| 杨丽蓉,赵红磊,赵海鹏,邱凯,陈燕,王明琪.HPLC-DAD/MS法测定抗风湿中成药中非法添加10种抗风湿化学成分[J].中国药品标准,2018,19(3):235-240 |
| HPLC-DAD/MS法测定抗风湿中成药中非法添加10种抗风湿化学成分 |
| Detection of Ten Antirheumatic Constituents Illegally Added in Chinese Patent Medicine by HPLC-DAD/MSYang Lirong1, Zhao Hongle11,Zhao Haipeng1, Qiu Kai1,Chen Yan1,Wang Mingqi2(1.Weifang Food and Drug Tests and Determines Center,Weifang 261200;2.Shandong Haiwang Pharmaceuticals Corporation,Jinan 250101) |
| 投稿时间：2018-03-07 修订日期：2018-06-08 |
| DOI： |
| 中文关键词: 高效液相色谱法 液质联用 中成药 抗风湿 非法添加 |
| 英文关键词: HPLC LC-MS Chinese patent medicine antirheumatic illegally added |
| 基金项目: |
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| 摘要点击次数: 659 |
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| 中文摘要: |
| 目的：建立检测抗风湿中成药中非法添加10种抗风湿化学成分的HPLC-DAD方法,并用MS/MS进行了化合物的归属分析。方法：用C18色谱柱(4.6mm×250mm,5um),以0.02mol/L乙酸铵(含0.05%乙酸)水溶液为流动相A,以乙腈为流动相B,梯度洗脱,波长240nm,流速1.0 ml/min,进行HPLC定性定量分析;再采用串联四级杆质谱的MRM模式检测,进行化合物归属分析,检测添加在中成药中的对乙酰氨基酚、甲氧苄啶、氨基比林、吡罗昔康、萘普生、双氯芬酸钠、醋酸泼尼松、吲哚美辛、保泰松、布洛芬10种化学成分。结果：10种抗风湿性化学成分液相检测的线性范围宽,相关性好,r≥0.9992,方法精密度的RSD为0.13%~0.45%；回收率在98.0%~100.9%之间；精密度、稳定性均符合要求；检测限为0.05~0.5 ug.ml<sub>-1</sub>；定量限为0.1~1.8 ug.ml<sub>-1</sub>。结论：本方法专属性强,操作简单,快捷,可作为中成药中非法添加以上10种抗风湿性化学成分的有效检测方法。 |
| 英文摘要: |
| Objective:To develop a HPLC-DAD method for determination of tenantirheumaticcconstituents illegally added inChinese patent medicine preparation,and a attribution analysis of related substances in the product by MS/MS．Methods:The analysis was performed on a C<sub>18</sub>column (4.6mm×250mm,5μm) with mobile phases A (0.02 mol/L ammonium acetate solution) and B (acetonitrile) by gradient elution at the flow rate of 1. 0 ml.min-1,and the detection wavelengthwas set at 240 nm．Multiple-reaction monitoring (MRM) was performed to identifyand quantifyparacetamol,trimethoprim,aminopyrine,piroxicam,naproxen,diclofenac sodium,prednisone acetate, |
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