HPLC kolonner I GC kolonner I SPE kolonner I Forbrugsvarer og tilbehør I Solvent saver I Kataloger

Acylation Reagents

Silane Surface-Coating Reagents

Silylation Reagents

Solvents

Specialized Reagents

High-purity silylation, alkylation and acylation reagents and labware for use in derivatization for drugs of abuse testing and other GC applications.

Acylation Reagents

Acylation is the conversion of compounds that contain active hydrogens (e.g., -OH, -SH and -NH) into esters, thioesters and amides, respectively, through the action of a carboxylic acid or a carboxylic acid derivative.

MBTFA (N-Methyl-bis[trifluoroacetamide])

For trifluoroacylating primary and secondary amines, hydroxyl and thiol groups under mild non-acidic conditions.

N-Methyl-bis(trifluoroacetamide) (MBTFA) trifluoroacetylates primary and secondary amines, hydroxyl and thiol groups under mild non-acidic conditions. The principal by-product from the derivatization reaction is N-methyltrifluoroacetamide, which is stable, volatile and does not present problems in subsequent gas chromatography. Sullivan and Schewe (1) have reported using MBTFA to prepare volatile TFA derivatives of mono-, di- and tri-saccharides with good yield. Subsequent gas chromatography showed excellent separations with retention times substantially lower than the corresponding TMS derivatives, for all compounds tested.

Highlights

• Trifluoroacetylates primary and secondary amines, as well as hydroxyl and thiol groups under mild nonacidic conditions
• Principal byproduct from the derivatization reaction is N-methyltrifluoroacetamide, which is stable, volatile and does not present problems in subsequent GC
• Produces very volatile derivatives of carbohydrates and can be used to selectively acylate amines in th presence of hydroxyl and carboxyl groups that have been protected by silyation
  

  
  References

   1. Sullivan, J. E., et al. (1977). Preparation and gas chromatography of highly volatile trifluoroacetylated carbohydrates using N-Methyl-bis(trifluoroacetamide). J. of Chromatography Science 15, 196. 
  

MBTFA (N-Methyl-bis[trifluoroacetamide])

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-49701	MBTFA	5 GM
TS-49703	MBTFA	25 ML
TS-49700	MBTFA	10 x 1 ML
TS-49704	MBTFA	100 ML

---

Perfluoro Acid Anhydrides (TFAA, PFAA and HFAA)

R	Name	M.W	bp	d.
CF3	TFAA	210.0	39.5-40.5°C	1.56
C2F5	PFAA	310.0	74°C	1.571
C3F7	HFAA	410.0	106-107°C	1.665

The most frequently used perfluoro acid anhydrides for preparing perfluoroacyl derivatives for GC/MS analysis are Trifluoroacetic Acid Anhydride (TFAA), Pentafluoropropionic Acid Anhydride (PFAA) and Heptafluorobutyric Acid Anhydride (HFAA). These reagents react readily with alcohols, phenols and amines to produce stable, volatile derivatives for TCD, FID and ECD techniques.

Highlights

• For preparation of perfluoroacyl derivatives for analysis by GC/MS
• React readily with alcohols, phenols and amines, producing stable volatile derivatives for TCD, FID and ECD techniques
• Produce corresponding perfluoro acid as a byproduct from the reaction with the active hydrogens from alcohols, phenols, mercaptans and amines
• Many compounds can be derivatized directly with anhydride and solvent; however, it is usually recommended that amine bases (such as triethylamine) be used to react with the acidic byproducts and drive the reaction toward completion
• Frequently used for drugs-of-abuse confirmation testing by GC/MS; TFAA is used to identify methamphetamine, PFAA is used to identify opiates and benzoylecgonine, and HFAA is used to identify amphetamines and phencyclidine

References TFAA

 1. Gilbert, R.B., et al. (1995). A labetalol metabolite with analytical characteristics resembling amphetamines. J. of Analytical Toxicology 19, 84.
 2. Verebey, K., et al. (1989). Rapid confirmation of enzyme multiplied immunoassay technique (EMITR) cocaine positive urine samples by capillary gas-liquid chromatography/nitrogen phosphorus detection (GLC/NPD). J. of Forensic Sciences 34, 46.
 3. Mule, S., et al. (1988). Confirmation and quantitation of cocaine, benzoylecgonine, ecgonine methyl ester in human urine by GC/MS. J. of Analytical Toxicology 12, 153.

References HFAA

 1. Jones, J.B., et al. (1993). A simple wash procedure for improving chromatography of HFAA derivatized amphetamine extracts for GC/MS analysis. J. of Analytical Toxicology 17, 447.

Perfluoro Acid Anhydrides (TFAA, PFAA and HFAA)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-63162	HFAA (Heptafluorobutyric Acid Anhydride)	100 gm
TS-63163	HFAA (Heptafluorobutyric Acid Anhydride)	25 gm
TS-63164	HFAA (Heptafluorobutyric Acid Anhydride)	10 x 1 ml
TS-65191	PFAA (Pentafluoropropionic Acid Anhydride)	100 gm
TS-65192	PFAA (Pentafluoropropionic Acid Anhydride)	25 gm
TS-65193	PFAA (Pentafluoropropionic Acid Anhydride)	10 x 1 ml
TS-67363	TFAA (Trifluoroacetic Acid Anhydride)	100 gm

---

Perfluoroacylimidazoles (TFAI and HFBI)

Offer effective acylation of hydroxyl groups, primary and secondary amines.

Properties of Perfluoroacylimidazoles
Name	R-Group	MW	Boiling Point	Density
TFAI	CF3	164.08	38-40°C/14mm	1.490
HFBI	C3F7	264.10	57-58°C/10mm	1.562

Highlights

• Offer considerable advantages over the anhydrides for the preparation of perfluoroacyl derivatives; the reactions are smooth, quantitative and produce no acid byproducts that must be removed from the system before injection
• Principal byproduct is imidazole (relatively inert)
• React with hydroxyl groups, primary and secondary amines, and quantitatively acylate indole alkylamines
• Tryptamine and metabolites present in spinal fluid have been analyzed by ECD using HFBI
• Used in bifunctional derivatization schemes and in exchange reactions where TMS derivitives are converted to HFB derivatives
• Hydroxyl groups of catecholamines are derivatized with TMSI, followed by conversion of the amines to acylamides with HFBI

* Perfluoroacylimidazoles are available in bulk quantities for manufacturing applications.

References

 1. Bennington, F., et.al. (1975). Identification and separation of indolealkylamines by gas-liquid chromatographic analysis of their heptafluorobutyryl derivatives.J. Chromatogr. 106:435-9.
 2. Seeley, S.D. and Powell, L.E. (1974). Gas chromatography and detection of microquantities of gibberellins and indoleacetic acid as their fluorinated derivatives. Anal. Biochem. 58:39-46.
 3. Horning, M.G., et.al. (1968). The GLC separation of hydroxyl-substituted amines of biological importance including the catecholamines. Preparation of derivatives for electron capture detection. Anal. Lett. 1(5):311-21.

Perfluoroacylimidazoles (TFAI and HFBI)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-44211	HFBI (Heptaflourobutyrylimidazole)	5 gm
TS-48882	TFAI (Trifluoroacetylimidazole)	10 x 1 ml

Alkylation Reagents

Used in derivatization for GC, alkylation represents the replacement of an active hydrogen by an aliphatic or aliphatic-aromatic (e.g., benzyl) group.

BF3-Methanol

A convenient methanol-catalyst system that quickly and quantitatively converts carboxylic acids to methyl esters.

BF3·Methanol - Quick Reference
Chemical Name:	BF3·Methanol
IUPAC Name:	trifluoroborane, methanol
Chemical Forumula:	CH40:BF3
Molecular Weight:	14% BF3 M.W. 67.82, 86% CH3OH M.W. 32.04
Boiling Point:	---
Density:	---

Highlights

• One of the most convenient reagents for fatty acid derivatization
• Provides a convenient methanol-catalyst system; when used in excess (with heating), quickly and quantitativly converts carboxylic acids to their methyl esters
• Used to prepare methyl esters directly from a variety of esters including glycerides
• Most suitable for derivatizing higher boiling carboxylic acids
• Most protocols require separation of the methyl ester from the reaction mixture by some form of extraction, followed by evaporation of the solvent
• Special techniques are required to obtain reproducible results from fatty acids below C8
• BF3 is a relatively strong Lewis acid—compounds that undergo reactions or rearrangements under acidic conditions should be derivatized with caution using this reagent

BF3-Methanol is one of the most convenient methods for the derivatization of fatty acids. Classical esterification chemistry calls for the reaction of a carboxylic acid with an alcohol in the presence of an acid catalyst. BF3-Methanol provides a convenient methanol-catalyst system which, when used in excess with heating, quickly and quantitatively converts carboxylic acids to their methyl esters. Similarly, this combination of methanol and strong acid can be used to prepare methyl esters directly from a variety of esters, including glycerides. As most protocols for preparation of methyl esters with BF3-Methanol require separation of the methyl ester from the reaction mixture by some form of extraction followed by evaporation of the solvent, this reagent is most suitable for derivatizing higher boiling carboxylic acids. Special techniques are required to obtain reproducible results from fatty acids below C8. BF3 is a relatively strong Lewis acid; therefore, compounds that undergo reactions or rearrangements under acidic conditions should be derivatized with caution when using this reagent.

BF3·Methanol

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-49370	BF3-Methanol	100 ML

---

MethElute Reagent (Trimethylanilinium Hydroxide [TMPAH])

The most volatile TMS-amide available, forms volatile and thermally stable derivatives for GC/MS applications.

TMPAH MethElute Reagent - Quick Reference
Chemical Name:	TMPAH Methelute
IUPAC Name:	trimethyl-phenyl-azanium hydroxide
Chemical Forumula:	C9H15NO
Molecular Weight:	153.2
Boiling Point:	11°C (Closed Cup)
Density:	N/A

Highlights

• 0.2M trimethylanilnium hydroxide in methanol
• For the quantitative methylation and detection of barbiturates, sedatives, xanthine bases, phenolic alkaloids and dilantin by GC
• Eliminates troublesome secondary peaks
• When the reagent is heated in the injector port of a gas chromatograph with drug-containing extracts of serum or urine, the drugs containing reactive amino, hydroxyl or carboxyl groups will be converted to the corresponding methyl derivatives; these volatile methylated drugs or metabolites then pass through the chromatograph for separation and quantitation

MethElute™ reagent is a 0.2 molar trimethylanilinium hydroxide in methanol solution. When heated with drug-containing extracts of serum or urine, those drugs containing reactive amino, hydroxyl and carboxy functions will be methylated at these reactive sites. These methylated drugs are then analyzed by gas chromatography.

MethElute Reagent (Trimethylanilinium Hydroxide [TMPAH])

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-49300	MethElute Reagent	10 ML
TS-49301	MethElute Reagent	12 x 1 ML

---

Methyl-8 Reagent (N,N-Dimethylformamide dimethyl acetal)

Easy and effective preparation of methyl esters from fatty acids and amino acids, phenols to methyl esters, thiols to mixed disulfides and certain diols to expides.

Methyl-8 Reagent - Quick Reference
Chemical Name:	N,N-Dimethylformamide dimethyl acetal
IUPAC Name:	N,N-dimethylformamide, 1,1-dimethoxyethane
Chemical Forumula:	C5H13NO2
Molecular Weight:	119.2
Boiling Point:	102 - 104°C
Density:	0.897

Highlights

• Rapidly and conveniently converts carboxylic acids to methyl esters, primary amines to N,N-dimethylaminoethylene derivatives, phenols to methyl eters, thiols to thioethers, and certain diols to epoxides
• Use with a solvent such as pyridine, DMF or acetonitrile; in most cases, reactions are repid, and quantitative yields are obtained as soon as the product/derivative is completely in solution

Methyl-8 Reagent offers significant advantages for preparing methyl esters for gas chromatography. The reaction is fast and complete upon dissolution. Yields are quantitative when reagent and sample are injected without prior mixing. Methyl-8 Reagent is packed in convenient, ready-to-use Hypo-Vial Sample Storage Vials and requires no water washing, extraction or concentration of the derivatives. In addition, no water is formed in the reaction. Reactions with Methyl-8 Reagent are usually complete upon dissolution. For long-chain solid acids, it is necessary to use Methyl-8 Reagent with additional solvent and mild heating, such as pyridine, benzene, methanol, chloroform, methylene chloride, THF and DMF.

References
  1. Zhang, Y., et al. (1993). Assay of the acetyl-CoA probe acetyl-sulfamethoxazole and of sulfamethoxazole by gas chromatography-mass spectrometry. Anal. Biochem. 212, 481.

Methyl-8 Reagent (N,N-Dimethylformamide dimethyl acetal)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-49350	Methyl-8 Reagent	25 ML

---

PFBBr (Pentafluorobenzyl Bromide)

Converts carboxylic acids, phenols, sulfonamides and mercaptans to halogenated derivatives that are easily detected by electron capture. PFBBr - Quick Reference Chemical Name: Pentafluorobenzyl bromide IUPAC Name: 1-(bromomethyl)-2,3,4,5,6-pentafluoro-benzene Chemical Forumula: C7H2BrF5 Molecular Weight: 260.9 Boiling Point: 174 - 175°C Density: 1.86

Highlights

• For the conversion of carboxylic acids, phenols, sulfonamides and mercaptans to halogenated derivatives that are easily detected by electron capture.
• Used to detect trace amounts of carboxylic acids, phenols and mercaptans in drinking water

Pentafluorobenzyl bromide (PFBBr), is used to convert carboxylic acids, phenols, sulfonamides and mercaptans to halogenated derivatives for electron capture detection (ECD) in GC analysis by an “extraction alkylation” technique. This process uses tetrabutylammonium as a counter ion and methylene chloride as a solvent. The use of PFBBr is ideal because reaction times are fast (~20 minutes) and derivatives are highly EC-sensitive, making them useful in low level determinations of fatty acids.

This reagent has been used with a potassium carbonate catalyst for the electron capture analysis of mercaptans, phenols and organic acids in surface water (1-3). PFBBr has been used in analyzing trace organics in asphalts as a “fingerprinting” technique for identifying asphalt pollutants found in surface water.

References
  1. Kawahara, F.K. (1968). Microdetermination of derivatives of phenols and mercaptans by means of electron capture gas chromatography. Anal. Chem.40:1009-10.
  2. Kawahara, F.K. (1968). Microdetermination of pentafluorobenzyl ester derivatives of organic acids by means of electron capture gas chromatography.Anal. Chem. 40:2073-5.
  3. Kawahara F.K. (1976). Trace organic components as fingerprints in gas chromatographic identification of spilled asphalt. Environ. Sci & Tech. 10:761-
  4. Bosin, T. R., et al. (1989). Harman in rat brain, lung and human CSF: effect of alcohol consumption. Alcohol 5: 505.
  5. Jones, A. B., (1981). Determination of cannabidol in plasma by electron-capture gas chromatography. J. Chromatography 226: 99.

PFBBr (Pentafluorobenzyl Bromide)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-58220	PFBBr	5 GM

---

Pentafluoropropanol (2,2,3,3,3-Pentafluoro-I-propanol)

Purified for GC-MS use.

Pentafluoropropanol is commonly used in combination with perfluoro acid anhydrides to make electron capture detection (ECD) derivatives for GC analysis to confirm the presence of drugs of abuse. Pentafluoropropionic acid anhydride (PFAA) is a perfluoro acid anhydride often used to prepare perfluoroacyl derivatives. This reagent reacts readily with alcohols, phenols and amines to produce stable, volatile derivatives for ECD and flame ionization detection (FID). However, adding fluorine atoms, such as Pentafluoropropanol, into compounds to be analyzed greatly enhances detection sensitivity.

• Purified for GC/MS use
• Adding fluorine atoms into compounds to be analyzed greatly enhances the sensitivity of certain detectors for those materials
• Used in ECD and GC-MS applications where it is advantageous to introduce fluorine atoms
• Carboxylic acids can be derivatized using a two-step reaction involving reaction with an anhydride, followed by a fluorinated alcohol

Pentafluoropropanol (2,2,3,3,3-Pentafluoro-I-propanol)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-65195	Pentafluoropropanol	10 x 1 ML

Silane Surface-Coating Reagents

Make glass and plastic surfaces inert and unreactive. Deactivate and recondition chromatographic columns.

AquaSil Siliconizing Fluid

Attaches the silane polymer, octadecyltrialkoxysilane, to make the surface inert or can polymerize to create an inert film.

Pierce multifunctional siliconizing fluids are specially designed to chemically bind microscopically thin, water-repellent films to glass, quartz, silica and ceramics. The coated surfaces are neutral, hydrophobic and non-oily. In addition, they offer increased resistivity and are not affected by solvents not readily hydrolyzed.

AquaSil Siliconizing Fluid is an easy-to-use silane monomer solution. It is supplied as a 20% solid solution in a mixture of diacetone alcohol and tertiary butyl alcohol. The primary silane component is an octadecyltrialkoxysilane, which, when mixed with water, is hydrolyzed to a silanol. This silanol condenses with available hydroxyl groups to form a film on the glass, plastic or ceramic surface. AquaSil Siliconizing Fluid is especially useful in the biochemical field because of its aqueous phase application to glass, plastic or ceramic and because of its strong resistance to base hydrolysis. CH3(CH2)16CH2Si(OR)3 Reasons to use Pierce AquaSil Siliconizing Fluid Easy to apply Water-dispersible Economical – a little goes a long way Surfaces can be recoated Improve water-repellency of coated surfaces Elimination of a meniscus Increase surface resistivity of coated surface Excellent lubricity Non-oily

AquaSil Siliconizing Fluid

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-42799	AquaSil Siliconizing Fluid	120 ML

---

Hexamethyldisilazane

HMDS greatly extends the practical range of GC, improving chromatographic results in the silylation of sugars and related substances.

HMDS - Quick Reference
Chemical Name:	Hexamethyldisilazane
IUPAC Name:	[dimethyl-(trimethylsilylamino)silyl]methane
Chemical Forumula:	C6H19NSi2
Molecular Weight:	161.4
Boiling Point:	125°C
Density:	0.77

Highlights

• Soluble in organic solvents
• Used for deactivating HPLC or GC packings and glass wool

Pierce HMDS is a popular monofunctional silane that many researchers have found useful for deactivating and coating HPLC or GC chromatographic supports. Because of their monofunctional nature, these silanes can react with only one site on the surface making the surface inert. Polymerization is not possible, eliminating the chances for unbound polymers to float free and elute from the column – avoiding exposure of unreacted silanols beneath the layer. In addition, surface moisture is eliminated, because monofunctional reagents dehydrate the surface. In addition to deactivation of glass surfaces, HMDS is a popular choice for silylation of sugars and related substances.

HMDS is also used for deactivating glass wool and for treating GC injection port glass inserts. Several methods are available for deactivating surfaces with HMDS. The item(s) to be deactivated may be dipped in a 5-10% solution of the reagent in a non-reactive solvent. Vapor phase deactivation may be performed by pulling straight vapor into an evacuated container containing the item to be deactivated. To deactivate glass wool, a few milliliters of HMDS may be added to a beaker along with the item and a watch glass placed on top of the beaker.

References
  1. Ren, S., et al. (1992). O-acetylated gangliosides in bovine buttermilk. Characterization of 7-O-acetyl, 9-O-acetyl, and 7,9-di-O-acetyl GD3. J. Biol. Chem. 267: 12632-12638.
  2. Footer, M and Bretscher, A. (1994). Brush border myosin-I microinjected into cultured cells is targeted to actincontaining surface structures. J. Cell Sci. 107: 1623-1631.
  3. Novina, R. (1982). Gas Liquid Chromatography of Isopropylidene Monosaccharides and their Trimethylsilyl Derivatives. Chromatographia 15: 241. 
  4. De Jong, A.P.J.M. et al. Derivatization of Catecholamines in Aqueous Solution for Quantitative Analysis in Biological Fluids. J. Chromatography, 276: 267. 
  5. Kotz, K.J. and McNiven, M.A. (1994). Intracellular Calcium and cAMP Regulate Directional Pigment Movements in Teleost Erythrophores. J. Cell Biol., 124(4): 463-474. 
  6. Mateo, R., et al. (1987). Capillary column gas chromatographic identification of sugars in honey s trimethylsilyl derivatives. J. Chromatography, 410: 319. 
  7. Suzuki, M., et al. (2005). Selected ion monitoring determination of acetylcholine during methoxypyridoxine seizures. Biol. Mass. Spec., 7(11-12): 537-539.

 

Hexamethyldisilazane

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-84769	Hexamethyldisilazane (HMDS)	100 g
TS-84770	Hexamethyldisilazane (HMDS)	25 g

---

SurfaSil Siliconizing Fluid

Attaches a short chain silane polymer to make the surface inert or can polymerize to create an inert film.

Pierce multifunctional siliconizing fluids are specially designed to chemically bind microscopically thin, water-repellent films to glass, quartz, silica and ceramics. The coated surfaces are neutral, hydrophobic and non-oily. In addition, they offer increased resistivity and are not affected by solvents not readily hydrolyzed.

SurfaSil Siliconizing Fluid is a short chain, clear polymeric silicone fluid consisting primarily of dichlorooctamethyltetrasiloxane. When applied to glass, quartz or similar materials, the unhydrolyzed chlorines present on the chain react with surface silanols to form a neutral, hydrophobic and tightly bonded film over the entire surface.

SurfaSil Siliconizing Fluid also works on metals, certain plastics, ceramics and fiber optics.

SurfaSil Siliconizing Fluid is acidic and care should be taken to avoid corrosion of metal that comes into contact with the liquid. The fluid is acidic only during application. After application the surface is neutral.

Reasons to use Pierce SurfaSil Siliconizing Fluid

• Easy to apply
• Soluble in organic solvents
• Economical – a little goes a long way
• Surfaces can be recoated
• Used to treat GC injection port glass inserts
• Improve water-repellency of coated surfaces
• Elimination of a meniscus
• Increase surface resistivity of coated surface
• Excellent lubricity
• Non-oily

SurfaSil Siliconizing Fluid

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-42800	Surfa-Sil Siliconizing Fluid	120 ml
TS-42801	Surfa-Sil Siliconizing Fluid	480 ml
TS-42855	Surfa-Sil Siliconizing Fluid	5 x 10 ml

Silylation Reagents

Reagents for the modification of active hydrogens from acids, alcohols, thiols, amines and other groups with an inert trimethylsilyl (TMS) group. Silylation adds mass and makes compounds more suitable for gas chromatography.

BSA (N,O-bis[Trimethylsilyl]acetamide)

Silylation reagent that reacts quantitatively under relatively mild conditions with a wide variety of compounds to form volatile, stable TMS derivatives.

BSA is the perfect reagent for volatile TMS derivatives. BSA reacts quantitatively using relatively mild conditions with a wide variety of compounds to form volatile, stable TMS derivatives for gas chromatograph analysis. BSA is used extensively for derivatizing alcohols, amines, carboxylic acids, phenols, steroids, biogenic amines and alkaloids; however, it is not recommended for use with carbohydrates or low molecular-weight compounds.

BSA - Quick Reference
Chemical Name:	N,O-bis[Trimethylsilyl]acetamide
IUPAC Name:	N-trimethylsilyl-1-trimethylsilyloxy-ethanimine
Chemical Forumula:	C8H21NOSi2
Molecular Weight:	199.1
Boiling Point:	71 - 73°C/35mm
Density:	0.832

Highlights

• Highly reactive trimethylsilyl donor that forms volatile, stable TMS derivatives
• Reacts quickly and quantitatively under mild conditions with a variety of compounds
• Derivatizes alcohols, amines, amides, carboxylic acids, phenols, steroids, biogenic amines and alkaloids

Applications

BSA is used with a solvent such as pyridine or DMF and reactions are generally rapid. When used with DMF, BSA is the most suitable reagent for derivatizing phenols. An impressive study of the silylating properties of BSA was conducted by Klebe, et al. that demonstrated the following reactions:

• Amino acids to form both N,O bonded TMS derivatives
• Hydroxyl compounds to form TMS ethers
• Organic acids to form TMS esters
• Aromatic amides to form N-TMS derivatives
• Applications for GC-MS, ECD, FID, GC-FTIR

References

 

1. Chambez, E.M. and Horning, E.C. (1968). Steroid trimethylsilyl ethers.Anal. Letters 1:201-11.
  2. Gehrke, C.W.,et al. (1970). Trimethylsilation of amino acids – Effect of solvents on derivatization using bis(trimethylsilyl)trifluoroacetamide.J.Chromatogr. 53:201.
  3. Gyllenhaal, O. and Hoffmann, K-J. (1984). Simultaneous determination of metoprolol and metabolites in urine by capillary column gas chromatography as oxazolidineone and trimethylsilyl derivatives. J. Chromatogr. 309:317-28.
  4. Kawashiro, K.,et al. (1984). Gas chromatography -mass spectrometry of trimethylsilyl derivatives of some iminodicarboxylic acids. Bull. Chem. Soc. Jpn. 57:2871-78.
  5. Klebe, J.F.,et al. (1966). Silylations with bis(trimethylsilyl)acetamide, a highly reactive silyl donor.JACS 88:3390-5.
  6. Laker, M.F. and Mount, J. (1980). Mannitol estimation in biological fluids by gas-liquid chromatography of trimethylsilyl derivatives. Clin. Chem. 2613:441-3.
  7. Lamkin, W.M.,et al. (1974). Analysis of methylthiohydantoins of amino acids by gas-liquid chromatography of their trimethylsilyl derivatives.Anal. Biochem. 58:422-38.
 8. Pang, H.,et al. (1982). Mass spectrometry of nucleic acid constituents. Trimethylsilyl derivatives of nucleosides. J. Org. Chem. 47:3923-32.
 9. Prater, W.A.,et al. (1980). Microanalysis of aqueous samples for phenols and organic acids.Anal. Lett. 13 (A3):205-12.
10. Sethi, S.k.,et al. (1983). Formation of a new derivative of secondary amines during trimethylsilylation with N,O-bis(trimethylsilyl)-fluoroacetamide. J. Chromatogr. 254:109-16.
11. Shieh, J.-J. and Desiderio, D. (1977). Derivatives for characterization of phosphoserine and phosphothreonine by gas chromatography – mass spectrometry.Anal. Lett. 10 (11):831-34.
12. Tai, S.S., et al. (1994). The certification of morphine and codeine in a human urine standard reference material. J. of Toxicology 18, 7.
13. Tanaka, A.et al. (1980). Gas chromatographic determination of nitrite in foods as trimethylsilyl derivative of 1H-benzotriazole.J. Chromatogr. 194:21-31.
14. Welch, M.J., et al. (1993). Hair analysis for drugs of abuse. J. of Toxicology 17, 389.

BSA (N,O-bis[Trimethylsilyl]acetamide)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-38836	BSA	10 x 1 ml
TS-38838	BSA	25 GM
TS-38839	BSA	100 GM

---

BSTFA (N,O-bis[Trimethylsilyl]trifluoroacetamide)

BSTFA - Quick Reference
Chemical Name:	N,O -Bis(trimethylsilyl)trifluoroacetamide
IUPAC Name:	2,2,2-trifluoro-N-trimethylsilyl-1-trimethylsilyloxy-ethanimine
Chemical Forumula:	C8H18F3NOSi2
Molecular Weight:	257.4
Boiling Point:	142°C
Density:	0.961 at 25°C

Highlights

• Trimethylsilyl donor strength approximately equal to BSA
• Increased volatility of reaction byproducts mono(trimethylsilyl)trifluoroacetamide and trifluoroacetamide, over corresponding nonfluorinated compounds from BSA
• Increased volatility makes it possible to derivatize smaller molecules with which the TMS derivatives elute with the byproducts from BSA
• React with the same classes of compounds as BSA, producing the same derivatives
• Add TMCS to derivatize amides, many secondary amines and hindered hydroxyls that are not derivatized by BSTFA alone

Applications

• Excellent derivatization reagent for analyzing drugs of abuse (THC Metabolites, Morphine and PCP)
• Can substitute for BSA in many derivatization techniques

BSTFA is an effective trimethylsilyl donor with donor strength approximately the same as its unfluorinated analog BSA, N,O-bis(trimethylsilyl)acetamide. It reacts with a wide range of polar compounds to replace labile hydrogens on a wide range of polar compounds with a -Si(CH3)3 group. Therefore, it is widely used to prepare volatile and thermally stable derivatives for gas chromatography and mass spectrometry.

One of the particular advantages of BSTFA over many of the other silylating reagents is the volatility of its by-products, mono (trimethylsilyl)trifluoro-acetamide and trifluoroac-etamide. For example, in the gas chromatographic analysis of some of the lower boiling TMS-amino acids and TMS-Krebs cycle acids, the retention times of these derivatives cause them to be co-eluted with the by-products from most TMS derivatization reagents. Good chromatographic separations can be obtained with BSTFA as the by-products from this reagent usually elute with the solvent front.

BSTFA can be used at full strength or diluted with a suitable solvent such as pyridine. In most applications it is advisable to use an excess of the silylating reagent and at least a two to one molar ratio of BSTFA to active hydrogen is recommended. Best results are obtained when the products of the silylation reaction are soluble in the final reaction mixture. Amides, many secondary amines and hindered hydroxyls will not be derivatized by BSTFA alone; however, when a catalyst such as trimethylchlorosilane is added, many of these compounds can be derivatized satisfactorily. A separate instruction book is available which addresses those applications which are best accomplished by the use of a catalyst with BSTFA.

References

 1. Bagnati, R., et al. (1996). Analysis of Dexamethasone and betamethasone in bovine urine by purification with an "on-line" immunoaffinity chromatography-high performance liquid chromatography system and determination by gas chromatography-mass spectrometry. Analytical Biochemistry 235, 119.
 2. Heinzen, H., et al. (1996). Mass Spectrometry of Labelled Triterpenoids: Thermospray and Electron Impact Ionization Analysis. Phytochemical Analysis 7(5), 237-244.
 3. Her, G.R., et al.(1985). Quantitative methodology for corticosteroids based on chemical oxidation using electrophilic products for electron capture-negative chemical ionization using capillary gas chromatography-mass spectrometry. Analytical Biochemistry 151, 292.
 4. Le Quéré, V., et al. (2004). Human CYP4F3s are the main catalysts in the oxidation of fatty acid epoxides. J. Lipid Res 45(8), 1446-1458.
 5. Nichols, F. C., et al. (2004). Structures and biological activities of novel phosphatidylethanolamine lipids of Porphyromonas gingivalis. J. Lipid Res 45(12), 2317-2330.
 6. Shanchun J., et al. (1994). Origins and simulated thermal alteration of sterols and keto-alcohols in deep sea marine sediments of the Okinawa Trough. Organic Geochemistry 21, 415.
 7. Yu, L., et al. (2005). Fine organic aerosols collected in a humid, rural location (Great Smoky Mountains, Tennessee, USA): Chemical and temporal characteristics. Atmospheric Environment 39(33), 6037-6050.

BSTFA (N,O-bis[Trimethylsilyl]trifluoroacetamide)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-38828	BSTFA	25 GM
TS-38829	BSTFA	100 GM
TS-38830	BSTFA	10 x 1 ML

---

BSTFA + TMCS

BSTFA - Quick Reference
Chemical Name:	N,O -Bis(trimethylsilyl)trifluoroacetamide
IUPAC Name:	2,2,2-trifluoro-N-trimethylsilyl-1-trimethylsilyloxy-ethanimine
Chemical Forumula:	C8H18F3NOSi2
Molecular Weight:	257.4
Boiling Point:	40°C/12mm
Density:	0.961

 

TMCS - Quick Reference
Chemical Name:	Trimethylchlorosilane
IUPAC Name:	chloro-trimethyl-silane
Chemical Forumula:	C3H9ClSi2
Molecular Weight:	108.7
Boiling Point:	57.6°C
Density:	0.858

Highlights

• Trimethylsilyl donor strength approximately equal to BSA
• Increased volatility of reaction byproducts mono(trimethylsilyl)trifluoroacetamide and trifluoroacetamide, over corresponding nonfluorinated compounds from BSA
• Increased volatility makes it possible to derivatize smaller molecules with which the TMS derivatives elute with the byproducts from BSA
• React with the same classes of compounds as BSA, producing the same derivatives

Applications

• Addition of 1% TMCS aids in derivatizing amides, many secondary amines and hindered hydroxyls that are not derivatized by BSTFA alone
• Excellent derivatization reagent for analyzing drugs of abuse (THC Metabolites, Morphine and PCP)
• Can substitute for BSA and BSA + 1 % TMCS in many derivatization techniques

BSTFA is an effective trimethylsilyl donor with donor strength approximately the same as its unfluorinated analog BSA, N,O-bis(trimethlysilyl)acetamide. It reacts with a wide range of polar compounds to replace labile hydrogens with a -Si(CH3)3 group. Therefore, it is used to prepare volatile and thermally stable derivatives for gas chromatography and mass spectrometry.

One of the particular advantages of BSTFA over many of the other silylating reagents is the volatility of its by-products, mono-(trimethylsilyl)trifluoro-acetamide and trifluoroacetamide. For example, in the gas chromatographic analysis of some of the lower boiling TMS-amino acids and TMS-Krebs cycle acids, the retention times of these derivatives cause them to be co-eluted with the by-products from most TMS derivatization reagents. Good chromatographic separations can be obtained with BSTFA, as the by-products from this reagent usually elute with the solvent front.

Amides, many secondary amines and hindered hydroxyls will not be derivatized completely by BSTFA alone; however, when a catalyst such as TMCS is added, many of these compounds can be derivatized satisfactorily. The mechanism for the catalytic effect of TMCS is not well understood; however, there is little doubt that the addition of the relatively weak silyl donor, TMCS, to BSTFA will enhance the donor strength of the stronger donor, BSTFA. The TMCS may participate through the formation of a reactive intermediate. Clearly, in those cases where amounts of TMCS up to 20% are used,7 the TMCS is not acting in a purely catalytic role.

The donor strengths of BSA and BSTFA are comparable and the reactivity enhancement from the addition of TMCS appears to be similarly comparable. Therefore, it is generally safe to assume that whenever a procedure calls for BSA + TMCS, BSTFA + TMCS can be substituted. This substitution is particularly appropriate when the peaks of interest have relatively low retention times and tend to be obscured by the derivatization reagent or the primary reaction products from the derivatization reagent. In some cases the combination of BSTFA and TMCS is a more powerful silyl donor than the comparable BSA and TMCS solution. In most cases the addition of 1% TMCS is sufficient to achieve the desired derivatization. If after using this reagent under forcing conditions (150°C for 12 hours) it appears that derivatization is not complete, additional TMCS may be added up to a final concentration of about 30%.

BSTFA + 1% TMCS or BSTFA + 10% TMCS can be used at full strength or diluted with a suitable solvent such as pyridine. In most applications it is advisable to use an excess of the silylating reagent, and at least a two to one molar ratio of BSTFA + TMCS per active hydrogen is recommended. Best results are obtained when the products of the silylation reaction are soluble in the final reaction mixture.

References

 1. Wang, W.L., et al. (1994). Simultaneous assay of cocaine, heroin and metabolites in hair, plasma, saliva and urine by gas chromatography-mass spectrometry. J. of Chromatography B 660, 279.
 2. Cone, E.J., et al. (1994). Simultaneous measurement of cocaine, cocaethylene, their metabolites, and “crack” pyrolysis products by gas chromatography-mass spectrometry. Clinical Chemistry 40(7), 1299.
 3. Dyer, R.G., et al. (1995). Simultaneous measurement of phytosterols (campesterol and ß-sitosterol) and 7-ketocholesterol in human lipoproteins by capillary column gas chromatography. Journal of Chromatography B 663, 1.
 4. Duez, P., et al. (1996). GC-MS profiling of urinary organic acids evaluated as a quantitative method. Clinical Chemistry, 42, 1609.
 5. Hocart, H.C., et al. (1986). Mass spectrometry and chromatography of t-Butyldimethylsilyl derivatives of cytokinin bases. Analytical Biochemistry, 153, 85.
 6. Heathers, G.P., et al. (1989). Anion exchange chromatographic separation of inositol phosphates and their quantification by gas chromatography. Analytical Biochemistry, 176, 109.
 7. Kemp, T.R., et al. (1982). High-resolution gas chromatography of methylated ribonucleosides and hypermodified adenosines.  Evaluation of trimethylsilyl derivatization and split and splitless operation modes. Journal of Chromatography, 241, 325.
 8. Sethi, S.K., et al. (1983). Formation of a new derivative of secondary amines during trimethylsilylation with n,o-bis(trimethylsilyl)-fluoroacetamide. N-(aminomethylene)-2,2,2-trifluoroacetamide. Journal of Chromatography, 254, 109.

BSTFA + TMCS

Product#	Description	Pkg. Size
TS-38440	BSTFA + 10% TMCS	10 x 1 ML	To order or get a price, please contact: info@md-scientific.dk
TS-38831	BSTFA + 1% TMCS	10 x 1 ML
TS-38832	BSTFA + 1% TMCS	10 GM
TS-38833	BSTFA + 1% TMCS	25 GM
TS-38834	BSTFA + 1% TMCS	100 GM

---

MOX Reagent (2% Methoxyamine?HCl in pyridine)

Useful for preparing oximes of steroids and ketoacids prior to silylation.

MOX Reagent converts keto groups to methoxime derivatives and prevents the formation of multiple derivatives when enols are present during silylation.

Highlights:

• 2% methoxyamine•HCl (MW 83.51) in pyridine
• Converts keto groups of steroids and ketoacids to methoxime derivatives
• Prevents formation of multiple derivatives when enols are present during silylation
• Supplied in Hypo-Vial Sample Storage Vial

References

 1. Horning, M.G., et al. (1968) Anal. Biochem. 22, 284.
 2. Chiabrando, C., et al. (1987). Anal. Biochem. 163, 255-262.

MOX Reagent (2% Methoxyamine•HCl in pyridine)

Product#	Description	Pkg. Size
TS-45950	MOX Reagent	10 ML	To order or get a price, please contact: info@md-scientific.dk

---

MTBSTFA (N-Methyl-N-[tert-butyldimethyl-silyl]trifluoroacetimide)

MTBSTFA - Quick Reference
Chemical Name:	N-Methyl-N-[tert-butyldimethyl-silyl]trifluoroacetimide
IUPAC Name:	N-(butyl-dimethyl-silyl)-2,2,2-trifluoro-N-methyl-acetamide
Chemical Forumula:	C9H18F3NOSi
Molecular Weight:	241.3
Boiling Point:	168-170°C
Density:	1.121

 

TBDMCS - Quick Reference
Chemical Name:	tert-Butyldimethylchlorosilane
IUPAC Name:	chloro-dimethyl-tert-butyl-silane
Chemical Forumula:	C6H15ClSi
Molecular Weight:	150.7
Boiling Point:	125°C
Density:	0.810

Highlights

• Derivatizes hydroxyl, carboxyl, thiol and primary and secondary amines
• Typical yields are >96%
• Provides TBDMCS ethers that are 104 times more stable to hydrolysis than TMS ethers
• Reaction byproducts are neutral and volatile
• Derivatives have a high molecular concentration at M-57
• Silylating potential increased by adding 1% TBDMCS

MBTSTFA and MBTSTFA + 1% TBDMCS convert hydroxyls, carboxyls, thiols and primary and secondary amines to TBDMS (tert-butyldimethylsilyl) derivatives, which are 10,000 times more stable than TMS ethers1. The reaction requires only 5 to 20 minutes to complete, and the by-products are neutral and volatile, preventing clogging of chromatography instruments. The addition of 1% TBDMCS acts as a catalyst, improving performance compared to MBTSTFA alone.

References

 1. Aponte, J.L., et al. (2001). Point mutations in the murine fumarylacetoacetate hydrolase gene: Animal models for the human genetic disorder hereditary tyrosinemia type 1. PNAS 98(2):641-645.
 2. Gloerich, J., et al. (2007). Metabolism of phytol to phytanic acid in the mouse, and the role of PPARa in it regulation. J. Lipid Res. 48:77-85.
 3. Janssen, D.J.M.T., et al. (2002). Surfactant phosphatidylcholine half-life and pool size measurements in premature baboons developing bronchopulmonary dysplasia.Pediat. Res. 52(5):724-9.
 4. Jenner, A.M., et al. (2002). Vitamin C protects against hypochlorous acid-induced glutathione depletion and DNA base and protein damage in human vascular smooth muscle cells. Arterioscler. Thromb. Vasc. Biol. 22(57):574-80.
 5. Kim, I., et al. (2002). Plasma and oral fluid pharmacokinetics and pharmacodynamics after oral codeine administration. Clin. Chem. 48(9):1486-96.
 6. Lehrmann, E., et al. (2003). Transcriptional profiling in the human prefontal cortex: Evidence for two activational states associated with cocaine abuse. Pharmacogenomics. 3(1):27-40.
 7. Oyler, J.M., et al. (2002). Duration of detectable methamphetamine and amphetamine excretion in urine after controlled oral administration of methamphetamine to humans. Clin. Chem. 48(10):1703-14.
 8. Rawlingson, A., et al. (2003). Functional significance of inducible nitric oxide synthase induction and protein nitration in the thermally injured cutaneous microvasculature. Am. Soc. Inv. Path. 162(4):1373-1380.
 9. Schepers, R.J.F., et al. (2003). Methamphetamine and amphetamine pharmacokinetics in oral fluid and plasma after controlled oral methamphetamine administration to human volunteers. Clin. Chem. 49(1):121-32.
10. Sewell, W.F., et al. (2005). Extracts of retina and brain that excite afferent fibers innervating hair cells contain a compound related to Hydroxyphenylglycine-N-carbamoyl. Synapse 58(2):129-140.
11. West, R.E., et al. (1993). GC/MS Analysis of five common benzodiazepine metabolites in urine as tert-butyl-dimethylsilyl derivatives. J. Anal. Tox. 17, 114.

MTBSTFA (N-Methyl-N-[tert-butyldimethyl-silyl]trifluoroacetimide)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-48920	MSTBSTFA	5 ml vial
TS-48927	MSTBSTFA + 1% TBDMCS	10 x 1 ml ampule

---

TMCS (Trimethylchlorosilane)

An excellent catalyst for difficult to silylate compounds.

TMCS - Quick Reference
Chemical Name:	Trimethylchlorosilane
IUPAC Name:	chloro-trimethyl-silane
Chemical Forumula:	C3H9ClSi2
Molecular Weight:	108.7
Boiling Point:	57.6°C
Density:	0.858

Highlights

• Excellent catalyst for compounds that are difficult to silylate
• Used to form trimethylsilyl esters of organic acids
• Addition of 1% TMCS aids in derivatizing amides, many secondary amines and hindered hydroxyls that are not derivatized by BSTFA alone

Monofunctional silanes are preferable for deactivating and coating chromatographic supports because they react with only one site on the surface. Polymerization is not possible and non-bound polymers will not float free and elute from the column, resulting in the subsequent exposure of non-reacted silanols beneath the layer. In addition, surface moisture is of no concern because monofunctional reagents dehydrate the surface.

There are several methods for deactivating surfaces with monofunctional reagents. Surfaces may be deactivated by slurrying or dipping the item(s) in a 5-10% solution of the reagent in a non-reactive solvent, pulling straight vapor into an evacuated container containing the item to be deactivated, or adding a few milliliters in a beaker along with the item and placing a watch glass on top, which is the method for glass wool silanization.

In addition to coating surfaces, TMCS is an excellent catalyst for difficult-to-silylate compounds. TMCS provides an excellent adjunct for forming trimethylsilyl ethers for GC determinations. In addition, it is used for preparing TMS derivatives of organic acids.

References

 1. Gholson, A.R., et al. (1987). Simultaneous ultrasonic extraction and silylation for determination of organic acids, alcohol, and phenols from airborne particulate matter. Journal - Association of Official Analytical Chemists, 70: 897.
 2. De Jong, A.P.J.M. et al. Derivatization of Catecholamines in Aqueous Solution for Quantitative Analysis in Biological Fluids. J. Chromatography, 276: 267.
 3. Novina, R. (1982). Gas Liquid Chromatography of Isopropylidene Monosaccharides and their Trimethylsilyl Derivatives. Chromatographia 15: 241.
 4. Wang, W.L., et al. (1994). Simultaneous assay of cocaine, heroin and metabolites in hair, plasma, saliva and urine by gas chromatography-mass spectrometry. J. Chromatography B 660: 279.
 5. Cone, E.J., et al. (1994). Simultaneous measurement of cocaine, cocaethylene, their metabolites, and “crack” pyrolysis products by gas chromatography-mass spectrometry. Clinical Chemistry, 40(7): 1299.
 6. Dyer, R.G., et al. (1995). Simultaneous measurement of phytosterols (campesterol and ß-sitosterol) and 7-ketocholesterol in human lipoproteins by capillary column gas chromatography. J. Chromatography B, 663: 1.
 7. Duez, P., et al. (1996). GC-MS profiling of urinary organic acids evaluated as a quantitative method. Clinical Chemistry, 42: 1609.
 8. Hocart, H.C., et al. (1986). Mass spectrometry and chromatography of t-Butyldimethylsilyl derivatives of cytokinin bases. Analytical Biochemistry, 153: 85.
 9. Heathers, G.P., et al. (1989). Anion exchange chromatographic separation of inositol phosphates and their quantification by gas chromatography. Analytical Biochemistry, 176: 109.
10. Kemp, T.R., et al. (1982). High-resolution gas chromatography of methylated ribonucleosides and hypermodified adenosines. Evaluation of trimethylsilyl derivatization and split and splitless operation modes. J. Chromatography, 241: 325.
11. Sethi, S.K., et al. (1983). Formation of a new derivative of secondary amines during trimethylsilylation with n,o-bis(trimethylsilyl)-fluoroacetamide. N-(aminomethylene)-2,2,2-trifluoroacetamide. J. Chromatography, 254: 109.

TMCS (Trimethylchlorosilane)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-88530	TMCS	25 GM

---

TMSI (N-Tremethylsilyimidazole)

The strongest silylation reagent for hydroxyls…reacts quickly and smoothly with hydroxyl and carboxyl groups.

TMSI is a derivatization reagent for the silylation of hydroxyl groups. This reagent reacts quickly and smoothly with hydroxyls and carboxylic acids, but not with amines. Because TMSI derivatives are less stable than TMS esters or ethers, TMSI is especially useful in multi-derivatization schemes for compounds containing both hydroxyl and amine groups.

TMSI is used in the derivatization of alcohols, phenols, organic acids, steroids, hormones, glycerols, nucleotides and narcotics. It is the strongest hydroxyl silylation reagent available for carbohydrates and steroids. TMSI is also excellent for C1 through C15 fatty acids in serum and urine.

Highlights

• Strongest reagent for silylation of hydroxyl groups; reacts quickly and smoothly with hydroxyl and carboxyl groups
• Does not react with amines or amides, making it possible to do multi-deratization for compounds containing both hydroxyl and amine groups
• Used for the silylation of sugars in the presence of small amounts of water; ideal for derivatizing sugars when they must be analyzed as syrups
• Derivatizes most steroid hydroxyls, including unhindered and highly hindered

References

 1. Yoo, Y., et al. (1995). Determination of nalbuphine in drug abuser’s urine. J. of Analytical Toxicology 19, 120.
 2. Seidel, V., et al. (1993). Analysis of trace levels of trichothecene mycotoxins in Austrian cereals by gas chromatography with electron capture detection. Chromatographia 37, 191.  
 3. Andrews, P.A., (1987). Silylated N,O-ketals fom the reaction of ketones with N-trimethylsilylimidazole. J. Chromatography, 419, 271.
 4. Masuda, S., et al. (1996). In Vitro Metabolism of the vitamin D Analog, 22-Oxacalcitriol, using cultured Osteosarcoma, Hepatoma, and Keratinocyte cell lines. J. Biol. Chem., 271 8700.
 5. Castagnetta, L., et al. (2002). Tissue content of hydroxyestrogens in relation to survival of breast cancer patients. Clinical Cancer Research, 8, 3146.
 6. Morineau, G., et al. (1997). Convenient chromatographic prepurification step before measurement of urinary cortisol by radioimmunoassay. Clinical Chemistry, 43, 786.
 7. Lu, H., et al. (1998). Effects of Phenobarbital on stereoselective metabolism of Ifosfamide in rats. Drug Metabolism and Disposition, 26, 476.

 

TMSI (N-Tremethylsilyimidazole)

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-88623	TMSI	10 x 1 ML
TS-88625	TMSI	25 GM
TS-88626	TMSI (N-Trimethylsilylimidazole)	4 x 25 gm

---

Tri-Sil BSA

BSA - Quick Reference
Chemical Name:	N,O-bis[Trimethylsilyl]acetamide
IUPAC Name:	N-trimethylsilyl-1-trimethylsilyloxy-ethanimine
Chemical Forumula:	C8H21NOSi2
Molecular Weight:	199.1
Boiling Point:	71 - 73°C/35mm
Density:	0.832

Pyridine - Quick Reference
Chemical Name:	pyridine
IUPAC Name:	pyridine
Chemical Forumula:	C5H5N
Molecular Weight:	79.1
Boiling Point:	115.2 - 115.3°C
Density:	0.983

Highlights

• BSA (2.5 mEq/ml*) in pyridine for one-step derivatizations (*1.25 mEq for amides)
• Derivatizes alcohols, phenols, organic acids, aromatic amides and amines
• Supplied in Hypo-Vial Sample Storage Vial

Applications

• Alcohols, phenols, some enols and other hydroxyl and polyhydroxyl compounds to from trimethylsilyl esters
• Organic acids to form trimethylsilyl esters
• Aromatic amides to form N-trimethylsilyl derivatives
• Amino acids to form both N- and O-trimethylsilyl derivatives
• Amines to form N-trimethylsilyl derivatives
• Not recommended for carbohydrates.

References

 1. Fennessey, P.V., et al. (1980). Org. Mass Spec. 15(4).
 2. Ramsdell, H.S., et al. (1980). J. Chromatogr. 181, 90-94.

Tri-Sil BSA

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-49012	Tri-Sil BSA in Pyridine	25 ml

---

Tri-Sil Concentrate

HMDS/TMCS (2:1) formulation without solvent.

 

Tri-Sil Concentrate

Product#	Description
TS-49005	Tri-Sil Concentrate	To order or get a price, please contact: info@md-scientific.dk

---

Tri-Sil Reagent

HMDS/TMCS in pyridine (2:1:10) mixture for one-step derivatization of organic hydroxyl and polyhydroxyl compounds into TMS ethers.

 

HMDS - Quick Reference
Chemical Name:	Hexamethyldisilazane
IUPAC Name:	[dimethyl-(trimethylsilylamino)silyl]methane
Chemical Forumula:	C6H19NSi2
Molecular Weight:	161.4
Boiling Point:	125°C
Density:	0.77

 

TMCS - Quick Reference
Chemical Name:	Trimethylchlorosilane
IUPAC Name:	chloro-trimethyl-silane
Chemical Forumula:	C3H9ClSi
Molecular Weight:	108.7
Boiling Point:	57.6°C
Density:	0.858

Highlights

• HMDS:TMCS:Pyridine (2:1:10) reagent-catalyst-solvent formulation for one-step derivatizations
• Derivatizes carbohydrates, phenols, steroids, sterols, organic acids, alcohols and some amines

Applications

The Pierce Tri-Sil Reagent is composed of HMDS, TMCS and high purity pyridine. It is useful for rapid production of TMS derivatives of polar compounds for gas chromatographic determination and biochemical synthesis. Tri-Sil Reagent is ideal for GC determination of the following:

• Sugars1,6
• Alcohols1
• Phenols7
• Steroids8,9
• Sterols10,11
• Bile acids and other organic acids12-14
• Some amines15-17

Tri-Sil Reagent is based on the procedure of Sweeley, et al.1 and is used for the optimal conversion of organic hydroxyland polyhydroxyl compounds into TMS ethers. The versatility, speed and ease of use of our Tri-Sil Reagent has made it the most widely used silylation formulation available.

Note: Not recommended for 3-ketosteroids

References

 1. Sweeley, C.C., et al. (1963). JACS 85: 2497.
 2. Hedgely, E.V. and Overend, W.G. (1960). Chem. and Ind. (London), 378.
 3. Ferrier, R.J. and Singelton, M.F. (1962). Tetrahedron 18: 1143.
 4. Ferrier, R.J. (1962). Ibid. 18: 1149.
 5. Sweeley, C.C. and Walker, B. (1964). Anal. Chem. 36:1461.
 6. Brower, H.E., et al. (1966). Anal. Chem. 38: 362.
 7. Langer, M., et al. (1958). Chem. And Ind. (London), 1664.
 8. Luukkainen, T., et al. (1960). Biochim. Biophys. Acta 52: 599.
 9. Miettinen, T.A., et al. (1965). J. Lipid Res. 6: 411.
10. Nair, P.P., et al. (1965). Anal. Chem. 37:631.
11. Rozanski, A. (1966). Anal. Chem. 38:36.
12. Makita, M. and Wells, W.W. (1963). Anal. Biochem. 5:523.
13. Burkhard, C.A. (1957). J. Org. Chem. 22:592.
14. Mehrotra, R.C. and Pant, B.C. (1963). J. Ind. Chem. Soc. 40:623.
15. Birkofer, L. and Ritter, A. (1960). Chem. Ber. 90: 424.
16. Horning, E.C., et al. (1964). Anal. Chem. 36: 1546.
17. Capella P. and Horning, E.C. (1966). Anal. Chem. 38: 316.
18. Betts, T.J., et al. (1984). J. Chrom. 291: 361.
19. Ng, L., et al. (1993). J. Chrom. 637: 104.

Tri-Sil Reagent

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-48999	Tri-Sil Reagent	10 x 1 ml
TS-49001	Tri-Sil Reagent	50 ml

---

Tri-Sil TBT

TMSI, BSA, TMCS (3:3:2) catalyzed silylation reagent formulation that converts all classes of hydroxyl groups to TMS ethers.

Product Detail
	TMSI - Quick Reference Chemical Name: N-Trimethylsilylimidazole IUPAC Name: imidazol-1-yl-trimethyl-silane Chemical Forumula: C6H12N2Si Molecular Weight: 140.3 Boiling Point: 99°C/14mm Hg Density: 0.957 BSA - Quick Reference Chemical Name: N,O-bis[Trimethylsilyl]acetamide IUPAC Name: N-trimethylsilyl-1-trimethylsilyloxy-ethanimine Chemical Forumula: C8H21NOSi2 Molecular Weight: 199.1 Boiling Point: 71 - 73°C/35mm Density: 0.832 TMCS - Quick Reference Chemical Name: Trimethylchlorosilane IUPAC Name: chloro-trimethyl-silane Chemical Forumula: C3H9ClSi Molecular Weight: 108.7 Boiling Point: 57.6°C Density: 0.858

Highlights

• TMSI:BSA:TMCS (3:3:2) reagent-catalyst formulation
• All classes of hydroxyl groups are converted to TMS ethers, including moderately hindered and unhindered hydroxyl groups

Tri-Sil TBT is a powerful catalyzed silylation reagent formulation that contains a 3:3:2 mixture of trimethylsilylimidazole (TMSI), N,O-bis-(trimethylsilyl)acetamide (BSA) and trimethylchlorosilane (TMCS). This reagent enables conversion of hydroxyls to trimethylsilyl derivatives. With proper selection of silylation reagents, unhindered, moderately-hindered and highly-hindered hydroxyls may be selectively silylated. BSA alone will silylate the unhindered 3a, 20a, and 21 hydroxyl groups on cortol (5b-pregnane-3a, 11ß, 17, 20a, 21-pentol); BSA with TMCS will silylate the aforementioned hydroxyls plus the moderately hindered 11b hydroxyl; and Tri-Sil TBT will silylate all five hydroxyls, including the highly-hindered 17a hydroxyl.

Note: When using a Tri-Sil TBT/dimethylformamide mixture, discard mixture after 12 hours.

References

 1. Seidel, V., et al. (1993). Chromatographia 37: 191-201.
 2. Mollica, J. A. and Strusz, R. F. (2006). Analysis of corticosteroid creams and ointments by high pressure liquid chromatography. J. Pharma. Sci 61(3): 444-47.
 3. Saisho, K., et. al. (2001). Hair Analysis for Pharmaceutical Drugs. II. Effective Extraction and Determination of Sildenafil and Its N-Desmethyl Metabolite in Rat and Human Hair by GC-MS. Biol. Pharm. Bull. 24(12): 1384—1388.
 4. Serdar, B., et. al. (2003). Urinary Biomarkers of Exposure to Jet Fuel (JP-8). Environ. Health Persp. 111: 1760-64.

Tri-Sil TBT

Product#	Description	Pkg. Size
TS-49016	Tri-Sil TBT	10 x 1 ML	To order or get a price, please contact: info@md-scientific.dk

---

 

Tri-Sil Z

TMSI in dry pyridine (1.5 mEq/ml) for derivatizing hydroxyl compounds, particularly carbohydrates.

Product Detail
	TMSI - Quick Reference Chemical Name: N-Trimethylsilylimidazole IUPAC Name: imidazol-1-yl-trimethyl-silane Chemical Forumula: C6H12N2Si Molecular Weight: 140.3 Boiling Point: 99°C/14mm Hg Density: 0.957 Pyridine - Quick Reference Chemical Name: pyridine IUPAC Name: pyridine Chemical Forumula: C5H5N Molecular Weight: 79.1 Boiling Point: 115.2-115.3°C Density: 0.983 Highlights TMSI:Pyridine (1:4) reagent-solvent formulation used for one-step derivatizations Derivatizes hydroxyl and polyhydroxyl compounds Will not derivatize amino groups Ideal for wet or dry carbohydrates Used to detect adulterated juices Tri-Sil Z is a mixture of trimethylsilylimidazole (TMSI) in dry pyridine (1.5 mEq/ml = 1 part TMSI: 4 parts pyridine) and is used primarily for derivatizing hydroxyl compounds, particularly carbohydrates, and does not react with amines. Tri-Sil Z can be used in the presence of water as long as there is enough reagent to react with both the water and the sample. The reagent reacts with water in a 2:1 ratio. Tri-Sil Z has been used successfully for the silylation of alcohols and phenols, nucleotides, indoles, glycols and polyglycols, amino acids, steroids, vitamins, organic acids, barbituarates, hydroxyl acids, flavonoids, carbohydrates, narcotics, hydroxylamines References  1. Low, N., et al. (1994). Normative data for commercial pineapple juice from concentrate. J. of AOAC International, 77, 965 .

Tri-Sil Z

Product#	Description	Pkg. Size
TS-49230	Tri-Sil Z	10 x 1 ML	To order or get a price, please contact: info@md-scientific.dk
TS-49231	Tri-Sil Z	25 ML

Solvents

Specially manufactured and packaged to meet the exact needs of silylation and other sensitive derivatization reactions.

Silylation Grade Solvents

Specially manufactured and packaged to meet the exact needs of siylation and other sensitive derivatization reactions.

Highlights

• Purified, dried and packaged under nitrogen in convenient Hypo-Vial Sample Storage Vials
• Use polar solvents (acetonitrile, dimethylformamide, dimethylsulfoxide, pyridine and tetrahydrofuran) to facilitate reactions; nonpolar organic solvent may be used, but they will not accelerate the rate of reaction
• Avoid water or alcohol because TMS reagents react with active hydrogen; avoid enolizable ketones
• Use dimethylformamide for steroids and other large molecules
• Use dimethylsulfoxide to prepare TMS derivatives of tertiary alcohols and some compound with reluctant solubility in other silylation solvents
• Pyridine is an excellent solvent and reaction medium for MS reactions and is an HCI acceptor in reactions involving organochlorosilanes
• Other commonly-used solvents include tetrahydrofuran and acetonitrile

* Dimethyl Sulfoxide is available in bulk quantities for manufacturing applications.

Silylation Grade Solvents

Product#	Description	Pkg. Size
TS-20062	Acetonitrile	50 ML	To order or get a price, please contact: info@md-scientific.dk
TS-20672	Dimethylformamide	50 ML
TS-20684	Dimethylsulfoxide	50 ML
TS-27530	Pyridine	50 ML
TS-27860	Tetrahydrofuran	50 ML

Specialized Reagents

Specialized reagents for GC applications.

Azomethine H Boron Reagent

Provides rapid, reliable and sensitive boron determination by colorimetry.

Azomethine H Boron Reagent provides fast, reliable and sensitive boron determination in soil, plants, composts, manure, water and nutrient solutions.

Advantages of Azomethine H over curcumin and other methods:

• Simplicity – fewer steps are involved in the analysisNonacid system; methods carried in water solution
• More accurate results obtained in plant analysis when compared to spectrographic data
• Essentially free from nitrate interference in soil samples with high nitrate levels
• Starting plant material digest or soil extract can be used to determine other important elements

References
  1. Basson, W.D., et al. (1969). Analyst 94, 1135-1141.
  2. John, M.K., et al. (1975). Anal. Lett. 8(8), 559-568.
  3. Gaines, T.P. and Mitchell, G.A. (1979). Comm. in Soil Sci. and Plant Anal. 10(8), 1099-1108.
  4. Wolf, B. (1971). Comm. in Soil Sci. and Plant Anal. 2(5), 363-374.
  5. DiLorenzo, A. (1973). J. Chromatogr. 75, 207-212.
  6. White, C.E., et al. (1947). Anal. Chem. 19, 802.

Azomethine H Boron Reagent

Product#	Description	Pkg. Size
			To order or get a price, please contact: info@md-scientific.dk
TS-40893	Azomethine H Boron Reagent	25 GM

---

 

MD Scientific ApS • Denmark • tlf. 7027 8565 • fax 7027 8566 • info@md-scientific.dk