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[摘要]
目的 建立抗风湿中成药中非法添加8种抗风湿性化学成分的UPLC-MS/MS检测方法。方法 以BEH-C18(100 mm×2.1 mm,1.7 μm)色谱柱分离,串联四级杆质谱仪检测,多反应监测(MRM)模式进行定性定量分析,样品以甲醇为溶剂超声提取,检测添加在中成药中的氢化可的松、地塞米松、醋酸泼尼松、对乙酰氨基酚、保泰松、萘普生、吡罗昔康与甲氧苄啶8种化学成分。结果 8种抗风湿性化学成分质谱检测的线性范围宽,相关性好,r2≥0.998 9;方法精密度的RSD为1.2%~3.5%;方法回收率为95.4%~104.9%;定量限为0.4~4.9 μg/mL;日内精密度的RSD为0.6%~2.7%(n=5),日间精密度的RSD为0.9%~2.9%(n=9)。结论 方法专属性强,操作简单快捷,可作为中成药中非法添加8种抗风湿性化学成分的有效检测方法。
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[Abstract]
Objective To develop a UPLC-MS/MS method for determination of eight antirheumatic cconstituents illegally added in Chinese patent medicine preparation. Methods The analysis was performed by a UPLC-MS/MS system of Waters Acquity UPLC/ Quattro Premier, with BEH-C18 (100 mm × 2.1 mm, 1.7 μm) column. Multiple-reaction monitoring (MRM) was performed to identify and quantify hydrocortisone, dexamethasone, prednisone 21-acetate, 4-acetamidophenol, phenylbutazone, naproxen, piroxicam, and trimethoprim, which were extracted with methanol by ultrasonic method. Results Eight linear calibration curves were obtained with r2 ≥ 0.998 9. The precision of the method was shown by RSD (n = 6) ranged from 1.2% to 3.5%. The recoveries were determinated at three concentration and ranged from 95.4% to 104.9%. The ranges of LLOQ were from 0.4 to 4.9 μg/mL and the RSDs (n = 9) of intra-day precision and inter-day precision were from 0.6% to 2.7% and from 0.9% to 2.9%. Conclusion The method is specific, simple, and fast to detect eight antirheumatic constituents illegally added in Chinese patent medicine preparation.
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