[关键词]
[摘要]
目的:首次建立气相色谱-质谱联用法(GC-MS)对鱼腥草鲜品挥发油中4-萜品醇、α-松油醇、乙酸龙脑酯和甲基正壬酮4 种成分的含量测定方法,为鱼腥草药材质量控制提供实验依据。方法:以内标物质为正十一碳烯,采用GC/MS法测定鲜品鱼腥草挥发油中4种成分的含量。气相色谱条件:程序升温条件:70℃持续5 min,5℃·min-1升温,140℃持续5 min,10℃·min-1升温,250℃持续10 min。进样口温度为230℃,载气为高纯He,流速为1.0 mL·min-1;分流比为10∶1;进样量为1 μL。质谱条件:检测器为MS,EI 为70EV,四极杆温度为150℃,离子源温度为230℃。结果:4-萜品醇、α-松油醇、乙酸龙脑酯和甲基正壬酮分别在6.492~129.84 μg·mL-1,1.097~21.944 μg·mL-1,12.128~242.56 μg·mL-1,84.76~169.52 μg·mL-1范围内线性关系良好。平均回收率分别为81.2%,80.6%,88.3%,84.6%;RSD 分别为1.5%,2.3%,1.1%,0.7%。结论:该法简便、灵敏、易操作,采用同时测定多指标成分评价鱼腥草质量,能有效的反映鱼腥草质量,可用于鲜鱼腥草药材的质量评价。
[Key word]
[Abstract]
This study was aimed to establish a method for assay of 4-terpineol, α-terpineol, bornyl acetate and methyl-n-nonylketone in Houttuynia cordata with gas chromatography-mass spectrometry (GS/MS) for the first time in order to provide experimental evidences for its quality control. Undecylen was analyzed quantitatively. GC/MS method was used in the content determination of 4 kinds of components in Houttuynia cordata. GC conditions were that the temperature was firstly increased to 70℃ for 5 min, and then 5℃·min-1 to 140℃ for 5 min. Then, the temperature was increased by 10℃·min-1 to 250℃ for 10 min. The temperature of the injection port was 230℃. The carrier gas was high purity helium. The flow rate was 1.0 mL·min-1. The split ratio was 10:1. The sample quantity was 1 μl. MS conditions were that the detector was MS, EI was 70ev, the temperature of four poles was 150℃, the temperature of ion source was 230℃. The results showed that there was good linearity of four components, which were 4-terpineol, α-terpineol, bornyl acetate and methyl-n-nonylketone obtained within the ranges of 6.492~129.84 μg·min-1, 1.097~21.944 μg·min-1, 12.128~242.56 μg·min-1, and 84.76~169.52 μg·min-1, respectively. The average recoveries of the four components were 81.2%, 80.6%, 88.3%, and 84.6%, respectively. The RSDs were 1.5%, 2.3%, 1.1%, and 0.7%, respectively. It was concluded that the method was simple, sensitive, and easy to operate. The simultaneous measurement of multiple indexes on the component for quality evaluation of Houttuynia cordata can effectively reflect the quality of Houttuynia cordata. It can also be used in the quality assessment of fresh Houttuynia cordate.
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[基金项目]
成都中医药大学基地建设项目(301301):四川美大康中药材种植有限责任公司鱼腥草GAP 基地建设,负责人:李敏。