GC法测定肠舒止泻制剂中两种挥发性成分
Simultaneous Determination of Two Volatile Components in Changshu Zhixie Preparations by GC
张珂 1曹玉 1黄丽梅1
作者信息
- 1. 南京市食品药品监督检验院,江苏 南京 210038
- 折叠
摘要
目的 建立气相色谱法测定肠舒止泻制剂中的乙酸龙脑酯、去氢木香内酯.方法 采用HP-INNOWax(30m×ϕ0.32 mm,0.25 μm)、FID 检测器,进样口温度 240.0℃,检测器温度 270.0℃.柱温初始温度为150.0℃,保持10 min,以20.0℃/min升至250.0℃,保持20 min;载气为高纯氦气,流速为1 mL/min;进样量1 μL,分流比10∶1;空气流量为400 mL/min,氢气燃气流量为30 mL/min,尾吹气流量为25 mL/min.结果 乙酸龙脑酯、去氢木香内酯的线性范围分别为3.287~525.893 μg/mL(r2=0.9998)、2.709~433.4423 μg/mL(r2=0.9999),平均回收率分别为94.13%、96.20%,RSD值分别为1.77%、1.23%.结论 气相色谱法测定肠舒止泻制剂中乙酸龙脑酯、去氢木香内酯时有效可靠,可用于肠舒止泻制剂的质量控制.
Abstract
(Objective)To establish a gas chromatography method for the simultaneous determination of bornyl acetate and dehydrocostus lactone in Changshu Zhixie preparations.(Methods)HP-INNOWax capillary column(30 m × ϕ0.32 mm,0.25 μm)was used as FID detector.The inlet temperature was 240.0 ℃,and the detector temperature was 270.0 ℃.The initial column temperature was maintained at 150 ℃ keep in 10 min,then increased to 250 ℃ at 20 ℃/min keep in 20 min.The gas was helium with a flow rate of 1 mL/min.The injection method was split injection with a split ratio of 10:1.The injection volume was 1 μL,and the air flow rate was 400 mL/min.The flow rate of hydrogen was 30 mL/min.The tail blowing flowrate was 25 mL/min.(Results)The linear ranges of bornyl acetate and dehydrocostus lactone were 3.287~525.893 μg/mL(r=0.9998)and 2.709~433.4423 μg/mL(r=0.9999)respectively,and the linear ranges were good in this range.The average recoveries were 94.13% and 96.20%,RSD were 1.84% and 1.36% respectively.(Conclusion)A gas chromatography method for simultaneous determination of bornyl acetate and dehydrocostus lactone in Changshu Zhixie preparations was established.The method is effective and reliable,and can be used to evaluate the quality control of Changshu Zhixie preparations.
关键词
气相色谱法/肠舒止泻制剂/去氢木香内酯/乙酸龙脑酯Key words
Gas chromatography/Changshu Zhixie preparations/Dehydrocostus lactone/Bornyl acetate引用本文复制引用
出版年
2024