摘要
目的：建立顶空固相微萃取-气相色谱法测定鱼腥草注射液中甲基正壬酮含量的方法，并与传统水蒸气蒸馏法提取结果进行比较。方法：采用固相微萃取器在样品瓶顶空吸附样品，对鱼腥草注射液样品进行提取，在气相色谱仪进样口高温下解吸附，并用毛细管气相色谱法分离甲基正壬酮。色谱柱为DB-1毛细管柱（30m×0．25mm，0．25μm）；载气：高纯氮（纯度≥99．999％）；柱温130℃；不分流进样，进样口温度200℃；FID检测器，温度200℃；流速1．0mL·min^-1。结果：甲基正壬酮在1．07～25．91μg呈良好线性关系，r=0．9996；平均加样回收率为99．77％，RSD=2．24％。含量测定结果与水蒸气蒸馏法（SD）无显著差异。结论：本方法简便、快速、准确、灵敏度高、重现性好，可取代SD—GC法用于鱼腥草注射液中甲基正壬酮的含量分析。
Objective： Methyl-n-nonylketone in Herba houttuyniae injection were extracted by HS-SPME and SD. The constituents were analyzed by GC spectrometry and compared. Methods： Herba houttuyniae injection samples were collected by a HS-SPME fiber and desported for 4 minutes at a high temperature in GC injector. Methyl-n-nonylketone were confirmed by capillary gas chromatography. The determination was performed on a DB-1 column （30m × 0.25mm, 0. 25μm） . Carrier gas was high purity nitrogen. The fopw rate was 1.0mL·min^-1. Temperature of column was 130℃. No spilt injection mode was used. Temperature of injector and FID detector were both 200℃ Results： A good linearity was obtained within the range of 1.07 - 25.91 μg （ r = 0. 999 6） . The average recovery of methyl-n-nonylketone was 99.77% （ RSD = 2.24% ） . Results of HS-SPME-GC method has no significant different with those of SD-GC. Conclusion： This method has been proved to be simple, rapid, accurate, high sensitivity and reproducible for the quality control of herba houttuyniae injection.
出处
《中国现代中药》
CAS
2008年第4期26-28,41,共4页
Modern Chinese Medicine
基金
陈可冀中西医结合发展基金
福建省高校中药学重点实验室开放课题基金资助项目(3000-905012020)
关键词
顶空固相微萃取
气相色谱法
鱼腥草注射液
甲基正壬酮
Head Space Solid-Phase Microextraction
Gas chromatography
Herba houttuyniae injection
Methyl-n-nonylketone
