Page 53 - 《中国药房》2022年12期

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

碱类成分 Δ

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晏 亮 ，丁银平 ，陈伟康 ，刘德鸿 ，李 晶（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
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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）
中图分类号 R927.2 文献标志码 A 文章编号 1001-0408（2022）12-1455-05
DOI 10.6039/j.issn.1001-0408.2022.12.08

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2 μL；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、5.36～6.32 μg/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。
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

Determination of four ephedrine components in Banxialu granules by QuEChERS combined with
UHPLC-MS/MS
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YAN Liang ，DING Yinping ，CHEN Weikang ，LIU Dehong ，LI Jing（1. Jiangxi Institute for Drug Control/
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NMPA Key Laboratory of Quality Evaluation of Chinese Patent Medicine/Jiangxi Province Engineering Research
Center of Drug and Medical Device Quality，Nanchang 330029，China；2. Jiangxi Provincial Institute of
Traditional Chinese Medicine，Nanchang 330029，China）
ABSTRACT 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 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，
Δ 基金项目：江西省中医药中青年骨干人才培养计划项目（No.赣
respectively. CONCLUSIONS Established method is simple，
中医药科教字〔2020〕2号）
＊副主任药师，硕士。研究方向：药物分析。E-mail：77416006@ rapid，sensitive and suitable for simultaneous determination of
qq.com 4 ephedrine components in Banxialu granules.
# 通信作者：主任中药师，硕士。研究方向：药物分析。电话： KEYWORDS Banxialu granules； ephedrine components；
0791-88158716。E-mail：13474608@qq.com QuEChERS；UHPLC-MS/MS；content determination

中国药房 2022年第33卷第12期 China Pharmacy 2022 Vol. 33 No. 12 ·1455 ·