GC Diagnostic Reagents BSTFA with 1% TMCS
Silylation derivatization reagent
TMCS enhances the reactivity of BSTFA for the silylation of difficult to derivatize compounds.
GC114 N,O-Bis(trimethylsilyl)trifluoroacetamide with 1% Trimethylchlorosilane , 99+%
[ 24589-78-4 ] f.w.:199.3daltons
b.p. 130-132; d. 1.075
- 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
The products are packaged in hypovials with septum inserts for ease in sampling and use.We manufacture these products so bulk quotations are always available with substantial savings.Each product is accompanied with a certificate of analysis including the GC chromatogram from QC.
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
- 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.
- 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.
- 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.
- Duez, P., et al. (1996). GC-MS profiling of urinary organic acids evaluated as a quantitative method. Clinical Chemistry, 42, 1609.
- Hocart, H.C., et al.(1986). Mass spectrometry and chromatography of t-Butyldimethylsilyl
derivatives of cytokinin bases. Analytical Biochemistry, 153, 85.
- Heathers, G.P., et al.(1989). Anion exchange chromatographic separation of inositol
phosphates and their quantification by gas chromatography.
Analytical Biochemistry, 176, 109.
- 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.
- 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.
| unit | price |
| 10gm | $48.00 |
| 25gm | $72.00 |
| 100gm | $179.00 |