Determination of the residues of bonded groups in silica gels for column chromatography by gas chromatography
Objective To determine the content of butyl(chloro)dimethylsilane in chromatographic silica gels by gas chromatography(GC).Methods GC with sample direct injection was adapted.The chromatographic column was a capillary column(HP-5,30 m×0.32 mm,0.25 μm)with 5%-diphenyl-95%dimethylsiloxane as the stationary phase,the carrier gas was N2,the temperature was programmed,the hydrogen flame ionization detector(FID)was used,the inlet temperature was 220℃,the detector temperature was 270℃,the carrier gas flow rate was 1.0 mL·min-1,the split ratio was 20∶1,and the injection volume was 1 μL.Results The specificity and the linear relationship of the standard curves were validated with the correlation coefficient r=0.999.The standard recovery rates were 98.57%-103.38%.The limit of detection(LOD)was 0.663 4 μg·mL-1,and the limit of quantitation(LOQ)was 2.211 2 μg·mL-1.Conclusion The method has the advantages of wide test range,accurate result,good repeatability and simple operation,and can meet the requirement of accurate detection of bonded group butyl(chloro)dimethyl silane residues in chromatographic silica gels.The study provides a basis for the effective control of tacrolimus quality and monomer residues from the source.
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