气相色谱法测定柱层析硅胶中键合基团的残留量

Determination of the residues of bonded groups in silica gels for column chromatography by gas chromatography

目的 建立气相色谱法(gas chromatography,GC)测定层析硅胶中键合基团正丁基二甲基氯硅烷的残留量。方法 采用GC直接进样。HP-5毛细管色谱柱(30 m×0.32 mm,0.25μm),固定液为5%-二苯基-95%二甲基硅氧烷,载气为氮气,程序升温,进样口温度为220℃,检测器为氢火焰离子化检测器(flame ionization detector,FID),检测器温度为270℃,载气流速为1.0 mL·min^(-1),分流比为20∶1,进样量为1μL。结果 该方法专属性良好,线性关系良好,相关系数r=0.999,加标回收率为98.57%~103.38%,检测限(limit of detection,LOD)为0.663 4μg·mL^(-1),定量限(limit of quantitation,LOQ)为2.211 2μg·mL^(-1)。结论 该方法测试范围宽,测定结果准确,重复性好,操作简单,可满足层析硅胶中键合基团正丁基二甲基氯硅烷残留的准确检测,为终产品他克莫司的质量控制提供依据。

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,0.25μm)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 1μL.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 0.6634μg·mL^(−1),and the limit of quantitation(LOQ)was 2.2112μg·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.