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

作　　者：尹金芳 周琴 苏万宝 海潇平 腾金梅 扎史永宗 熊华斌 李晓芬 高云涛 YIN Jin-fang;ZHOU Qin;SU Wan-bao;HAI Xiao-ping;TENG Jin-mei;Zha-Shi-Yong-Zong;XIONG Hua-bin;LI Xiao-fen;GAO Yun-tao(Yunnan Minzu University School of Chemistry and Environment,Kunming 650500,China;National Local Joint Engineering Research Center of Bio Based Materials Green Preparation Technology,Kunming 650500,China)

机构地区：[1]云南民族大学化学与环境学院,昆明650500 [2]生物基材料绿色制备技术国家地方联合工程研究中心,昆明650500

出　　处：《药物分析杂志》2023年第8期1343-1351,共9页Chinese Journal of Pharmaceutical Analysis

基　　金：国家自然基金(21367025);云南省科技计划项目(2017FD118)。

摘　　要：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

关 键 词：疏风解毒胶囊 QUECHERS 单萜 气相色谱-质谱联用 气相色谱 乙酸乙酯 Α-蒎烯 Β-蒎烯 (-)-萜烯-4-醇 γ-松油烯 

分 类 号：R917[医药卫生—药物分析学]