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(4.6 mm×250 mm,5μm),以0.02 mol·L^(-1)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240 nm,流速1.0 mL·min^(-1),进行HPLC定性定量分析;再采用串联四极杆质谱的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≥0.999 2,方法精密度符合要求;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0.05~0.5μg·mL^(-1);定量限为0.1~1.8μg·mL^(-1)。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。
Objective: To establish an HPLC-DAD method for determination of 10 antirheumatic components illegally added in Chinese patent medicines with MS/MS attribution analysis for these components. Methods: The test was performed in C18 column(4.6mm×250mm,5μm) under the gradient elution with mobile phase A(0.02mol·L^-1 ammonium acetate 5% acetic acid solution) and mobile phase B (acetonitrile). The flow rate was 1. 0mL·min^-1, and the detection wavelength was 240 nm. Multiple-reaction monitoring(MRM) mode of tandem quadru- pole mass spectrometry was adopted to identify paracetamol, trimethoprim, aminopyrine, piroxieam, naproxen, diclofenac sodium, prednisone acetate, indomethacin, phenylbutazone and ibuprofen. Results: There were the wide linear ranges with r≥0. 999 7 for 10 antirheumatic components. The precision of the method met the criteria, and the recoveries of 10 components fell into 98.0% to 100. 9%. The precision and stability data met the requirements. The limits of detection fell into 0. 05 μg·mL^-1 to 0. 5 μg·mL^-1, and the limits of quantitation fell into 0. 1μg·mL^-1 to 1.8 μg·mL^-1. Conclusion: The established method has the good specificity, and it is simple. It can be applicable to determination of 10 antirheumatic components illegally added in Chinese patent medicines.
作者
杨丽蓉
赵红磊
赵海鹏
邱凯
陈燕
王明琪
YANG Lirong;ZHAO Honglei;ZHAO Haipeng;QIU Kai;CHEN Yan;Wang Mingqi(Weifang Institute for Food and Drug Control, Weifang 261200, China;Shandong Haiwang Pharmaceutical Corporation, Jinan 250101, China)
出处
《中国药品标准》
CAS
2018年第3期235-240,共6页
Drug Standards of China