QuEChERS结合UHPLC-MS/MS法测定半夏露颗粒中4种麻黄碱类成分
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篇名: QuEChERS结合UHPLC-MS/MS法测定半夏露颗粒中4种麻黄碱类成分
TITLE: Determination of four ephedrine components in Banxialu granules by QuEChERS combined with UHPLC-MS/MS
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AgilentXDB-C18为色谱柱,以5mmol/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0.40mL/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/z166.2→148.1(麻黄碱、伪麻黄碱)、m/z152.2→134.1(去甲伪麻黄碱)、m/z180.2→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、1.99~59.83ng/mL(r>0.99),检测限分别为0.41、0.42、0.39、0.60ng/mL,定量限分别为1.38、1.41、1.29、1.99ng/mL;精密度、稳定性(48h)、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。
ABSTRACT: OBJECTIVE To establish the met hod for the purific ation 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-C 18 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 mL/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/mL,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.
期刊: 2022年第33卷第12期
作者: 晏亮,丁银平,陈伟康,刘德鸿,李晶
AUTHORS: YAN Liang,DING Yinping ,CHEN Weikang ,LIU Dehong ,LI Jing
关键字: 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
KEYWORDS: Banxialu granules ; ephedrine components ;
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