顶空气相色谱法测定市售56批次强力枇杷露中薄荷脑的含量

Content Determination of Menthol in 56 Batches of Qiangli Pipa Syrup by HS-GC

目的：建立测定强力枇杷露中薄荷脑含量的方法,并对市售56批次强力枇杷露中薄荷脑的含量进行测定。方法：采用顶空气相色谱法。色谱柱为Agilent HP-INNOWAX毛细管柱,柱温采用恒温130℃（保持7 min）,检测器为氢火焰离子化检测器,进样口温度为200℃,检测器温度为250℃,载气为高纯氮气,流速为3 ml/min,分流比为10∶1,进样量为1 000μl。结果：薄荷脑质量浓度在0.007 07～0.141 40 mg/ml范围内与峰面积呈良好的线性关系（r=0.999 1）;精密度、稳定性、重复性试验的RSD≤3.37%;加样回收率为94.3%～99.6%（RSD=1.86%,n=6）。56批次强力枇杷露中薄荷脑的含量差异较大。结论：该方法操作简单、精密度好、准确可靠,可用于强力枇杷露中薄荷脑的含量测定。抽样结果表明,有必要更新该制剂的含量检测项目,加强对其质量控制。

OBJECTIVE： To establish the HS-GC method for the content determination of menthol in Qiangli Pipa syrup, and the content of menthol in 56 batches of Qiangli Pipa syrup commercially available was determined. METHODS： HS-GC was per- formed on the column of Agilent HP-1NNOWAX, column temperature was 130℃（maintaining 7 min）, FID was used as detector, inlet temperature was 200 %, detector temperature was 250 %, carrier gas was high-purity nitrogen, flow rate was 3 ml/min, split ratio was 10：1 and the injection volume was 1 000 μl. RESULTS： The linear range of menthol was 0.007 07-0.141 40 mg/ml（r= 0.999 1）;RSDs of precision, reproducibility and stability tests were no more than 3.37%; average recovery was 94.3%-99.6% （RSD=1.86%, n=6）. There was significant difference in the contents of menthol in 56 batches Qiangli Pipa syrup. CONCLU- SIONS： The method is simple, sensitive, accurate and reliable, and can be used for content determination of menthol in Qiangli Pi- pa syrup. The sampling results show it is necessary to update the detecting items for the content of Qiangli pipa loquat and strength- en the quality control of it.