气相色谱法测定枇杷止咳颗粒中薄荷脑含量

Content Determination of Menthol in Pipa Zhike Granules by Gas Chromatography

目的 建立测定枇杷止咳颗粒中薄荷脑含量的气相色谱法。方法 以萘为内标物,色谱柱为DB-WAX毛细管柱(30 m×0.32 mm,0.25μm),检测器为氢火焰离子化检测器,柱温为120℃,进样口、检测器温度均为250℃,空气流速为400 mL/min,氢气流速为30 mL/min,流速为3 mL/min,分流比为10∶1,进样量为1μL。结果 薄荷脑质量浓度在1.05×10^(-3)-0.209 mg/mL范围内与对照品峰面积/萘峰面积线性关系良好;精密度、重复性、稳定性试验结果的RSD均小于1.0%;平均加样回收率为86.52%,RSD为2.36%(n=6)。5家生产企业9批样品含量为每袋0.600-1.125 mg。结论 所建方法简便、快速,可用于枇杷止咳颗粒中薄荷脑含量的测定。

Objective To establish a gas chromatography(GC) method for the content determination of menthol in Pipa Zhike Granules.Methods Naphthalene was used as the internal standard,and the chromatographic column was DB-WAX capillary column(30 m × 0. 32 mm,0. 25 μm),the detector was a hydrogen flame ionization detector(FID),the column temperature was 120 ℃,the temperature of the sample inlet and the detector was 250 ℃,the flow rate of air was 400 mL/min,the flow rate of hydrogen was 30 mL/min,the split ratio was 10∶1,and the injection volume was 1 μL.Results The linear range of menthol was 1. 05 × 10^(-3)-0. 209 mg/mL. The RSDs of precision,repeatability and stability tests were all less than 1. 0%. The average recovery of menthol was 86. 52% with an RSD of 2. 36%(n = 6). The content of nine batches of samples from five manufacturers was in the range of 0. 600-1. 125 mg per bag.Conclusion The method is simple and rapid,which can be used for the content determination of menthol in Pipa Zhike Granules.