改进的微型化QuEChERS-GC/GC-MS法测定疏风解毒胶囊中4个挥发单萜含量

Determination of four monoterpenes in Shufeng Jiedu capsules by miniaturized QuEChERS-GC/GC-MS

目的:针对中药挥发性成分GC-MS或气相色谱测定前提取净化需要,设计并制作了新型微型化QuEChERS装置。建立的微型化QuEChERS-GC-MS对疏风解毒胶囊进行定性半定量分析,并建立测定疏风解毒胶囊挥发油中α-蒎烯、β-蒎烯、γ-松油烯和(-)-萜烯-4-醇4个成分的GC定量分析方法。方法:通过漩涡提取中药挥发性成分,采用新型微型化QuEChERS净化装置进行净化,结合GC-MS对疏风解毒胶囊的化学成分进行鉴定,其含量采用GC外标法测定。色谱条件:GC-MS采用DB-WAX毛细管色谱柱(30 m×0.25 m,0.25μm);GC采用SH-Rtx-1毛细管色谱柱(30.0 m×0.25 mm,0.25μm),进样口温度为250℃,流速为1.0 mL·min^(-1),分流比为10∶1;载气为高纯度氦气(纯度>99.999%),进样量为1.0μL;升温程序:初始温度为80℃,保持3 min,后以10℃·min^(-1)速率升至250℃,保留为5 min。结果:从疏风解毒胶囊共鉴定出24个挥发性成分,单萜类物质占50%以上。含量测定中选择4个主要活性单萜成分,4个成分进样浓度在测定范围内线性关系良好,精密度、稳定性和重复性良好,平均回收率(n=3)为80%~120%。3份样品中α-蒎烯、β-蒎烯、γ-松油烯和(-)-萜烯-4-醇的含量(n=3)分别为0.0075、0.0960、0.0214和0.0497 mg·g^(-1)。结论:本文的微型化QuEChERS装置避免了过程挥发性成分损失,净化性能高,微量化速度快,有效改善中药挥发成分分析结果的准确性和精密性。

Objective:To designe and manufacture a new miniaturized device of QuEChERS for the needs of extraction and purification during the pretreatment of volatile components of Chinese medicines.The established of miniaturized QuEChERS-GC-MS was applied for qualitative and semi quantitative analysis of Shufeng Jiedu capsules.On this basis,to establish a quantitative analysis method for the four components(α-Pinene,β-Pi⁃nene,γ-terpinene and(-)-terpene-4-alcohol)in the volatile oil of Shufeng Jiedu capsules.Methods:Extraction of volatile components from traditional Chinese medicine was by vortex.Purification was per⁃formed by using a novel miniaturized device of QuEChERS.The chemical constituents of Shufeng Jiedu capsules were identified by GC-MS.The content of Shufeng Jiedu capsules was determined by external standard method by GC.GC-MS was performed on a DB-WAX Capillary column(30 m×0.25 m,0.25μm film thickness).GC was performed on a SH-Rtx-1 Capillary column(30 m×0.25 m,0.25μm film thickness).The injector temperature was 250℃.The carrier gas flow rate was 1.0 mL·min^(-1).The split ratio was 10∶1,and high purity helium(purity>99.999%)was used.The injection volume was 1.0μL.The oven temperature procedure:the initial temperature was maintained at 80℃for 3 min,after 250℃at the rate of 10℃·min^(-1)for 5 min.Results:A total of 24 volatile components were identified in Shufeng Jiedu capsules.Monoterpene account for more than 50%,and four main active monoterpenes were selected in the content determination.The injection con⁃centration of the 4 ingredients had a good linear relationship within the determination range.The precision,stabil⁃ity and repeatability of the experiment were well.And the average recovery rate(n=3)was within 80%-120%.The contents ofα-pinene in three samples was 0.0075 mg·g^(-1),the content ofβ-pinene in three samples was 0.0960 mg·g^(-1),the content ofγ-terpinene in three samples was 0.0214 mg·g^(-1),and the content of(-)-terpene-4-alcohol in three samples was 0.0497 mg·g^(-1).Conclusion:The miniaturized device of QuEChERS avoids the loss of volatile components during the process in this paper,which has high purification performance,miniaturized and fast.The accuracy and precision of volatile components analysis results of tradition⁃al Chinese medicine is effectively improve.