QuEChERS结合UHPLC-MS/MS法测定半夏露颗粒中4种麻黄碱类成分  

Determination of four ephedrine components in Banxialu granules by QuEChERS combined with UHPLC-MS/MS

作　　者：晏亮 丁银平 陈伟康 刘德鸿 李晶[2] YAN Liang;DING Yinping;CHEN Weikang;LIU Dehong;LI Jing(Jiangxi Institute for Drug Control/NMPA Key Laboratory of Quality Evaluation of Chinese Patent Medicine/Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang 330029,China;Jiangxi Provincial Institute of Traditional Chinese Medicine,Nanchang 330029,China)

机构地区：[1]江西省药品检验检测研究院/国家药品监督管理局中成药质量评价重点实验室/江西省药品医疗器械质量工程研究中心,南昌330029 [2]江西省中医药研究院,南昌330029

出　　处：《中国药房》2022年第12期1455-1459,共5页China Pharmacy

基　　金：江西省中医药中青年骨干人才培养计划项目(No.赣中医药科教字[2020]2号)。

摘　　要：目的建立半夏露颗粒供试品的净化方法,并检测其中麻黄碱、伪麻黄碱、去甲伪麻黄碱、甲基麻黄碱4种麻黄碱类成分的含量。方法3批半夏露颗粒以含1%甲酸的甲醇提取,再经含N-丙基乙二胺吸附剂(PSA)和十八烷基键合硅胶吸附剂(C18)的QuEChERS方法进行前处理,并采用超高效液相色谱-串联三重四极杆质谱法测定,以Agilent XDB-C18为色谱柱,以5 mmol/L乙酸铵溶液(含0.1%甲酸)-乙腈为流动相进行梯度洗脱,流速为0.40 mL/min,柱温为30℃,进样量为2μL;采用电喷雾离子源,以多反应监测模式进行正离子扫描,用于定量分析的离子对分别为m/z 166.2→148.1(麻黄碱、伪麻黄碱)、m/z 152.2→134.1(去甲伪麻黄碱)、m/z 180.2→162.2(甲基麻黄碱)。结果采用QuEChERS净化方法所得供试品溶液澄清近无色。麻黄碱、伪麻黄碱、去甲伪麻黄碱、甲基麻黄碱检测质量浓度的线性范围分别为1.38~206.82、1.41~212.13、1.29~19.34、1.99~59.83 ng/mL(r>0.99),检测限分别为0.41、0.42、0.39、0.60 ng/mL,定量限分别为1.38、1.41、1.29、1.99 ng/mL;精密度、稳定性(48 h)、重复性试验的RSD均小于2%;平均加样回收率为95.75%~100.87%(RSD<2%,n=9);上述4种麻黄碱类成分的含量分别为20.62~26.02、20.96~24.90、2.26~2.63、5.36~6.32μg/g。结论所建立的方法简便、快速、灵敏,适用于半夏露颗粒中4种麻黄碱类成分的同时检测。OBJECTIVE To establish the method for the purification of test sample of Banxialu granules,and to determine the contents of 4 ephedrine components such as ephedrine,pseudoephedrine,norpseudoephedrine and methylephedrine. METHODS Three batches of Banxialu granules were extracted with methanol(containing 1% formic acid) and pretreated with QuEChERS method of N-propyl ethylenediamine adsorbent(PSA)and octadecyl bonded silica gel adsorbent(C18). Ultra high performance liquid chromatography tandem triple quadrupole mass spectrometry(UHPLC-MS/MS)was adopted. The separation was performed on an Agilent XDB-C18 column with 5 mmol/L ammonium acetate solution(containing 0.1% formic acid)-acetonitrile as mobile phase(gradient elution)at the flow rate of 0.40 m L/min. The column temperature was set at 30 ℃,and sample size was 2 μL. The electrospray ionization source was adopted,and positive ion scanning was performed in multiple reaction monitoring mode. The ion pairs used for quantitative analysis were m/z 166.2→148.1(ephedrine,pseudoephedrine),m/z 152.2→134.1(norpseudoephedrine),m/z 180.2→162.2(methylephedrine). RESULTS The solution obtained by QuEChERS purification method was clear and nearly colorless. The linear ranges of ephedrine,pseudoephedrine,norpseudoephedrine and methylephedrine were 1.38-206.82,1.41-212.13,1.29-19.34,1.99-59.83 ng/mL(r>0.99). The limits of detection were 0.41,0.42,0.39 and 0.60 ng/mL. The limits of quantitation were 1.38,1.41,1.29 and 1.99 ng/m L,respectively. RSDs of precision,stability(48 h)and repeatability tests were all lower than 2%. The average recoveries were 95.75%-100.87%(RSD<2%,n=9). The contents of above 4 ephedrine components were 20.62-26.02,20.96-24.90,2.26-2.63,5.36-6.32 μg/g, respectively. CONCLUSIONS Established method is simple, rapid, sensitive and suitable for simultaneous determination of 4 ephedrine components in Banxialu granules.

关 键 词：半夏露颗粒 麻黄碱类成分 QuEChERS方法 超高效液相色谱-串联三重四极杆质谱法 含量测定 

分 类 号：R927.2[医药卫生—药学]