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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 ； |
| 阅读数： | 184 次 |
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