GC Derivatizing Reagents

For GC analysis, the substance to be analyzed must be in the gaseous form. Because of this, the analysis of many organic compounds requires that injections, columns, and detectors are kept at relatively high temperatures. However, many organic compounds are thermally unstable. In such cases, it is necessary to convert the substance to be analyzed to a more volatile derivative appropriate for GC analysis. GC derivatizing reagents such as silylating, acylating, and alkylating reagents are used for this conversion.
Meanwhile, GC has been used for the analysis of biogenic substances. This generally requires the use of various derivatizing reagents. As an example, trimethylsulfonium hydroxide 1 can easily convert fatty acids, fatty acid esters, and glycerides into their methyl esters in a single step through the pyrolysis of the corresponding sulfonium salts 2.1) The low-boiling by-product, dimethyl sulfide, does not disturb the chromatographic separation of the samples. Therefore, the method using 1 is suitable for detection not only of longer chain fatty acids but also of relatively short chain fatty acids. 1 has been successfully applied for sample preparation in the analysis of fatty acids in microorganisms and human blood serum.2)

■Typical Procedure
A mixture of 1mg of fatty acids is dissolved in 0.1mL toluene, and then 0.5mL trimethylsulfonium hydroxide 1 (0.2mol/L methanol solution) is added. After 30 min at room temperature, the solution is used for gas chromatography.

Silylation

Esterification & Alkylation

Acylation

Others

Silylation

Trimethylsilylation

H0089 H0089 A5601 A5601 A5603 A5603
B3402 B3402 C0306 C0306 B0510 B0510
B0511 B0511 B0830 B0830 T0492 T0492
T0591 T0591 M0959 M0959 M0536 M0536
M1059 M1059 M0672 M0672 T0590 T0590
T0585 T0585 A5602 A5602 A5604 A5604
A5605 A5605
H0089 1,1,1,3,3,3-Hexamethyldisilazane
A5601 BSA [=N,O-Bis(trimethylsilyl)acetamide] [for Gas Chromatography]
A5603 BSTFA [=N,O-Bis(trimethylsilyl)trifluoroacetamide] [for Gas Chromatography]
B3402 BSTFA-TMCS (99:1) [Derivatizing Reagent for GC]
C0306 Chlorotrimethylsilane
B0510 N,O-Bis(trimethylsilyl)acetamide (25% in Acetonitrile) [Trimethylsilylating Reagent, for NH2 compounds]
B0511 N,O-Bis(trimethylsilyl)acetamide
B0830 N,O-Bis(trimethylsilyl)trifluoroacetamide
T0492 N-(Trimethylsilyl)diethylamine
T0591 N-(Trimethylsilyl)dimethylamine
M0959 N-Methoxy-N,O-bis(trimethylsilyl)carbamate [Simultaneous silylation and methoximation reagent for GC]
M0536 N-Methyl-N-trimethylsilylacetamide [Trimethylsilylating Agent]
M1059 N-Methyl-N-trimethylsilylheptafluorobutyramide [TMS Reagent for GC using FID]
M0672 N-Methyl-N-trimethylsilyltrifluoroacetamide [Trimethylsilylating Agent]
T0590 N-Trimethylsilylacetamide
T0585 N-Trimethylsilylimidazole [Trimethylsilylating Reagent]
S0162 SILREST [Column conditioner for Gas chromatography]
A5602 TMS-BA [=N,O-Bis(trimethylsilyl)acetamide] (25% in Acetonitrile) [for Gas Chromatography]
A5604 TMS-HT (HMDS and TMCS in Anhydrous Pyridine) [for Gas Chromatography]
T0274 TMS-HT (HMDS and TMCS in Anhydrous Pyridine) [Trimethylsilylating Reagent, for OH compounds]
A5605 TMS-Imidazole (=N-Trimethylsilylimidazole) [for Gas Chromatography]
T0623 TMS-PZ [Trimethylsilylating Reagent, for wet or dry Sugars, Mono or Poly Saccharides]

Five species of A5601, A5602, A5603, A5604, and A5605 are trimethylsilylating reagents prepared under strict quality control for highly sensitive analysis. They are purified and controlled so that impure substances having high boiling points, which are detrimental to the analysis, are below 20ppm per one component.

Dimethylsilylation

T0833 T0833 C0778 C0778
T0833 1,1,3,3-Tetramethyldisilazane
C0778 Chlorodimethylsilane

Alkyldimethylsilylation

D1516 D1516 D1596 D1596 D1572 D1572
B1043 B1043 D1590 D1590 D0135 D0135
D1594 D1594 B1906 B1906 B1150 B1150
B0995 B0995
D1516 1-(Dimethylethylsilyl)imidazole [Dimethylethylsilylating Agent]
D1596 1-(Dimethylisopropylsilyl)imidazole [Dimethylisopropylsilylating Agent]
D1572 1-(Dimethylpropylsilyl)imidazole [Dimethylpropylsilylating Agent]
B1043 1-(tert-Butyldimethylsilyl)imidazole [tert-Butyldimethylsilylating Agent]
D1590 Chlorodimethylpropylsilane [Dimethylpropylsilylating Agent]
D0135 Dimethylethylchlorosilane [Dimethylethylsilylating Agent]
D1594 Dimethylisopropylchlorosilane [Dimethylisopropylsilylating Agent]
B1906 N,O-Bis(tert-butyldimethylsilyl)acetamide [tert-Butyldimethylsilylating Agent]
B1150 N-(tert-Butyldimethylsilyl)-N-methyltrifluoroacetamide
B0995 tert-Butyldimethylchlorosilane [tert-Butyldimethylsilylating Agent]

Halomethylsilylation

B0847 B0847 C0605 C0605 B0990 B0990
B0847 (Bromomethyl)chlorodimethylsilane
C0605 (Chloromethyl)dimethylchlorosilane
B0990 1,3-Bis(chloromethyl)tetramethyldisilazane

Others

D1816 D1816 A1275 A1275 D1976 D1976
B1435 B1435 P0854 P0854 P0908 P0908
D1816 1,3-Diphenyltetramethyldisilazane
A1275 Allylchlorodimethylsilane [Allyldimethylsilylating Reagent for GC/MS]
D1976 Dichlorodiethylsilane
B1435 N,O-Bis(diethylhydrogensilyl)trifluoroacetamide [Simultaneous cyclic silylene and silyl derivatizing reagent for GC]
P0854 Pentafluorophenyldimethylchlorosilane [Pentafluorophenyldimethylsilylating Agent]
P0908 Pentafluorophenyldimethylsilyldiethylamine [Pentafluorophenyldimethylsilylating Agent]

Esterification & Alkylation

N,N-Dimethylformamide Dialkyl Acetals

D1303 D1303 D1302 D1302 D1294 D1294
D1332 D1332 D2071 D2071 D1595 D1595
D1301 D1301
D1303 N,N-Dimethylformamide Di-tert-butyl Acetal [for Esterification]
D1302 N,N-Dimethylformamide Dibutyl Acetal [for Esterification]
D1294 N,N-Dimethylformamide Diethyl Acetal [for Esterification]
D1332 N,N-Dimethylformamide Dimethyl Acetal [for Esterification] (0.5ml*10)
D2071 N,N-Dimethylformamide Dimethyl Acetal [for Esterification]
D1595 N,N-Dimethylformamide Dineopentyl Acetal [for Esterification]
D1301 N,N-Dimethylformamide Dipropyl Acetal [for Esterification]

Triazenes

B0949 B0949 M0641 M0641
B0949 1-Benzyl-3-p-tolyltriazene [for Esterification]
M0641 1-Methyl-3-p-tolyltriazene [for Esterification]

Onium Hydroxides

T0961 T0961 T0676 T0676 T1460 T1460
P0245 P0245 T1576 T1576
T0961 3-(Trifluoromethyl)phenyltrimethylammonium Hydroxide (5% in Methanol) [for Transesterification of Glyceride]
T0676 Tetramethylammonium Hydroxide (10% in Methanol)
T1460 Tetramethylammonium Hydroxide (ca. 25% in Water)
P0245 Trimethylphenylammonium Hydroxide (20-25% in Methanol) [for On-Column Methylation]
T1576 Trimethylsulfonium Hydroxide (0.2mol/L in Methanol) [Methylating Reagent]

BCl3, BF3, HCl-Alkanol Solutions

X0033 X0033 X0034 X0034 X0035 X0035
X0036 X0036 X0037 X0037
X0033 Boron Trichloride - Methanol Reagent (5-10%) [for Esterification] (1ml*10)
X0034 Boron Trifluoride - Butanol Reagent (10-20%) [for Esterification] (1ml*10)
X0035 Boron Trifluoride - Isopropyl Alcohol Reagent (10-20%) [for Esterification] (1ml*10)
X0036 Boron Trifluoride - Methanol Reagent (10-20%) [for Esterification] (1ml*10)
X0037 Boron Trifluoride - Propanol Reagent (10-20%) [for Esterification] (1ml*10)
X0039 Hydrogen Chloride - Butanol Reagent (5-10%) [for Esterification] (1ml*10)
X0038 Hydrogen Chloride - Methanol Reagent (5-10%) [for Esterification] (1ml*10)
X0041 Hydrogen Chloride - Methanol Reagent (5-10%) [for Esterification]

Diazomethane Precursors & Equivalents

M0527 M0527 N0265 N0265 T1146 T1146
M0527 1-Methyl-3-nitro-1-nitrosoguanidine (wetted with ca. 50% Water, containing 5g on a dry weight basis)
N0265 N-Methyl-N-nitrosourethane
T1146 Trimethylsilyldiazomethane (ca. 10% in Hexane, ca. 0.6mol/L)

Acylation

H0467 H0467 T0670 T0670 B0986 B0986
H0024 H0024 H0337 H0337 A0694 A0694
M0671 M0671 P0807 P0807 P0566 P0566
T0433 T0433
H0467 1-(Heptafluorobutyryl)imidazole [Acylating Agent]
T0670 1-(Trifluoroacetyl)imidazole
B0986 Bistrifluoroacetamide
H0024 Heptafluorobutyric Acid
H0337 Heptafluorobutyric Anhydride
A0694 N-Acetylimidazole
M0671 N-Methylbis(trifluoroacetamide) [Trifluoroacylating Agent]
P0807 Pentafluorobenzoyl Chloride
P0566 Pentafluoropropionic Anhydride
T0433 Trifluoroacetic Anhydride

Others

B0529 B0529 F0280 F0280 P0822 P0822
P0809 P0809 B0857 B0857
B0529 Butylboronic Acid (contains varying amounts of Anhydride) [for Esterification]
F0280 Ferroceneboronic Acid (contains varying amounts of Anhydride) [Cyclic boronating reagent for GC/MS]
P0822 O-(2,3,4,5,6-Pentafluorobenzyl)hydroxylamine Hydrochloride [for Oxime Preparation]
P0809 Pentafluorobenzyl Bromide
B0857 Phenylboronic Acid (contains varying amounts of Anhydride)

Literature

1) W. Butte, J. Chromatogr. 1983, 261, 142 [DOI].
2) K.-D. Müller, H. P. Nalik, E. N. Schmid, H. Husmann, G. Schomburg, J. High. Resolut. Chromatogr. 1993, 16, 161; K.-D. Müller, H. Husmann, H. P. Nalik, G. Schomburg, Chromatographia 1990, 30, 245 [DOI]; L. Akoto, R. Pel, H. Irth, U. A. T. Brinkman, R. J. J. Vreuls, J. Anal. Appl. Pyrolysis 2005, 73, 69 [DOI].


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