| 引用本文: | 励炯,林伟杰,王红青,邱红钰,诸葛陇.HPLC-MS/MS测定动物源性中药中的3种β2-受体激动剂残留[J].中国现代应用药学,2018,35(4):501-505. |
| Li Jiong,Lin Weijie,Wang Hongqing,Qiu Hongyu,ZhuGe long.Detection of 3 β2-agonists Residues in Animal-derived Chinese Medicine by HPLC-MS/MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2018,35(4):501-505. |
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| 摘要: |
| 目的 建立动物源性中药中的克伦特罗、沙丁胺醇和莱克多巴胺3种β2-受体激动剂残留的高效液相色谱-串联四级杆质谱（HPLC-MS/MS）检测方法。方法 以Agilent XDB-C18（50 mm×4.6 mm，5.0µm）色谱柱分离，串联四级杆质谱仪检测，MRM模式进行定性定量检测分析，样品经酶解后，经MCX固相萃取柱净化，检测阿胶和人工牛黄中的克伦特罗、沙丁胺醇和莱克多巴胺。结果 3种β2-受体激动剂质谱检测的线性范围宽，相关性好，R2 ≥ 0.997 1；方法精密度RSD为1.4%~2.3%（n=6）；方法回收率范围为89.4%~102.8%；定量限范围为0.25~5.50µg·L-1；日内精密度为2.4%~4.6%（n=5），日间精密度为1.9%~3.7%（n=9）。结论 本方法专属性强，操作简单、快捷，可作为动物源性中药中克伦特罗、沙丁胺醇和莱克多巴胺3种β2-受体激动剂残留的定量、定性的有效检测方法。 |
| 关键词: 动物源 阿胶 人工牛黄 三重四级杆 高效液相色谱法 β2-受体激动剂 |
| DOI：10.13748/j.cnki.issn1007-7693.2018.04.010 |
| 分类号:R917.101 |
| 基金项目: |
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| Detection of 3 β2-agonists Residues in Animal-derived Chinese Medicine by HPLC-MS/MS |
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Li Jiong, Lin Weijie, Wang Hongqing, Qiu Hongyu, ZhuGe long
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Hangzhou Institute for Food and Drug Control, Hangzhou 310017, china
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| Abstract: |
| OBJECTIVE To develop an high performance liquid chromatography with triple quadrupole mass spectrometry (HPLC-MS/MS) method to determine 3 β2-agonists including clenbuterol, salbutamol and ractopamine in animal-derived Chinese medicine. METHODS The analysis was performed by a HPLC-MS/MS system with Agilent XDB-C18(50 mm×4.6 mm, 5.0 µm) column. Multiple-reaction monitoring (MRM) was performed to identify and quantify 3 β2-agonists, which were extracted from Asini Colla Corii and Bovis Calculus Artifactus, purified with MCX SPE columns. RESULTS three linear calibration curves were obtained with R2 ≥ 0.997 1. The precision of the method were showed by RSD (n=6) ranged from 1.4% to 2.3%. The recoveries were determinated at three concentrations and ranged from 89.4% to 102.8%. The ranges of LOQ were from 0.25 µg·L-1 to 5.50 µg·L-1, and the RSDs of intra-day precision (n=5) and inter-day precision (n=9) were from 2.4% to 4.6% and from 1.9% to 3.7%. CONCLUSION The method is specific, simple and fast to detect the 3 β2-agonists in animal-derived Chinese medicine. |
| Key words: animal-derived Asini Colla Corii Bovis Calculus Artifactus triple quadrupole HPLC β2-agonists |
