顶空单滴微萃取-气相色谱法在鱼腥草注射液挥发性成分分析中的应用

Application of Headspace Single Drop Microextrction Coupled with Gas Chromatography in Determination of Volatile Component in Houttuynia cordata Injection

目的探讨顶空单滴微萃取-气相色谱法在鱼腥草注射液中甲基正壬酮、4-萜烯醇、月桂烯含量的测定。方法精密吸取样品的甲醇溶液10μL注入盛有5 mL水的鱼腥草注射液样品瓶中,以1.5μLN,N-二甲基甲酰胺为萃取溶液（含内标苯甲醇）,萃取温度为60℃、萃取时间为5 min,萃取后直接吸回0.5μL进行GC分析检测,测定甲基正壬酮、4-萜烯醇、月桂烯的含量。采用30 m×0.53 mm PEG毛细管柱,FID检测器,程序升温。结果甲基正壬酮、4-萜烯醇、月桂烯分别在5~85μg·mL-1（r1=0.999 3）、10~135μg·mL-1（r2=0.999 4）和10~180μg·mL-1（r3=0.999 5）范围内呈良好线性关系;平均加样回收率分别为100.3%、98.7%、99.4%,RSD分别为2.7%、3.0%、2.5%。结论顶空单滴微萃取-气相色谱法操作简单,结果准确,灵敏度高,可推广用于鱼腥草注射液挥发性成分含量的测定。

Objective A simple, fast gas chromatography method based on headspace single drop microextraction was used for the determination of three kinds of volatile components of methyl-n-nonylketone, 4-terpineol and myrcene in Houttuynia cordata injection, Methods A special sample pretreatment method was performed by adding 10μL methanol solution into 5 mL water ofHouttuynia cordata injection sample in a caped 10 mL sample, 1.5 μL microdrop of N, N-dimethylfo rmamide with benzy alcoho as internal standard was formed on the pinpoint of microsy tinge needle, exposing 5 rain at extraction temperature of 60℃. After extraction, 0.5μL of extract was directely injected into GC for analysis to the determination of methyl-n-nonylketone, 4-terpineol and myrcene. The determination was carried out on a capillary column （ 0.53 mm ×30 m ） with PEG as the stationary phase with FID as the detector. A temperature programme was employed. Results The excellent separation and detection of the target components was accomplished. The calibration curves were lined in the range of 5- 85μg.mL-1 （ r1 = 0.999 3）, 10- 135×g.mL-1 （ rE = 0.999 4） and 10- 180μg.mL-1 （ r3 = 0.999 5）, respectively.The average recoveries of methyl-n-nonylketone, 4-terpineol, and myrcene varied 100.3%, 98.7% and 99.4%, and RSD were 2.7%, 3.0%, 2.5%, respectively. Conclusion The proposed method was proved to be simple, fast, and accurate without complicated sample pretreatment. It was expected to be widely applied for the analysis of volatile components in traditional Chinese medicines.