He Xiaowen, Jiang Ye, Lei Lili
Department of Pharmacy, HeBei Medical University, Shijiazhuang 050017, China.
Zhongguo Zhong Yao Za Zhi. 2010 Oct;35(20):2718-21.
A simple, fast GC method based on headspace single drop microextraction (HS-SDME) was used for the determination of menthol and methyl salicylate in Baicao oils. A special sample pretreatment method was performed by adding 10 microL the oil its methanol solution into 5 mL water in a caped 10 mL sample vial, a 1.5 microL microdrop of N,N-dimethylformamide with benzyl alcohol as internal standard was formed on the pinpoint of microsyringe needle, exposing 5 min at extraction temperature of 40 degrees C. After extraction, 0.5 microL of extract was directely injected into GC for analysis. The determination was carried out on a capillary column (0.53 mm x 30 m) with PEG as the stationary phase with FID as the detector. A temperature programm was employed. The excellent separation and detection of the target components was accomplished. The average recoveries varied between 95.4% and 99.2%, and relative standard deviations were less than 1.9%. The calibration curves were linear in the range of 1.26-80.5 mg x L(-1) for menthol (r = 0.999 0) and 2.49-1.59 x 10(2) mg x L(-1) for methyl salicylate (r = 0.999 1), respectively. The proposed method is proved to be simple, fast, accurate and low cost without complicated sample pretreatment HS-SDME is expected to be widely applied for the analysis of volatile components in traditional Chinese medicines.
建立了一种基于顶空单滴微萃取(HS-SDME)的简单、快速气相色谱(GC)法,用于测定百草油中的薄荷醇和水杨酸甲酯。采用特殊的样品前处理方法,将10 μL百草油的甲醇溶液加入到10 mL带盖样品瓶中的5 mL水中,在微量注射器针尖上形成1.5 μL含苯甲醇作为内标的N,N-二甲基甲酰胺微滴,于40℃萃取温度下暴露5 min。萃取后,将0.5 μL萃取液直接注入GC进行分析。测定在以聚乙二醇(PEG)为固定相的毛细管柱(0.53 mm×30 m)上进行,采用氢火焰离子化检测器(FID)。采用程序升温。实现了目标成分的良好分离与检测。平均回收率在95.4%至99.2%之间,相对标准偏差小于1.9%。薄荷醇的校准曲线在1.26 - 80.5 mg·L⁻¹范围内呈线性(r = 0.999 0),水杨酸甲酯的校准曲线在2.49 - 1.59×10² mg·L⁻¹范围内呈线性(r = 0.999 1)。该方法无需复杂的样品前处理,具有简单、快速、准确、低成本的特点,HS-SDME有望广泛应用于中药挥发性成分的分析。