首页|LC-MS/MS法测定消肿止痛酊中马兜铃酸Ⅰ的含量

LC-MS/MS法测定消肿止痛酊中马兜铃酸Ⅰ的含量

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目的 建立消肿止痛酊中马兜铃酸Ⅰ的专属性检测方法,为消肿止痛酊的质量安全控制提供理论依据。方法 通过液相色谱-质谱联用法对消肿止痛酊中的马兜铃酸Ⅰ进行含量测定。采用Poroshell 120 SB-C18(2。1 mm × 100 mm,2。7 μ m)色谱柱进行分离,以0。1%甲酸溶液(含5 mmol/L甲酸铵)-乙腈为流动相进行梯度洗脱,柱温30℃,流速0。3 ml/min,在电喷雾离子化正离子模式下,进行多反应检测,外标法定量。结果 马兜铃酸Ⅰ在0。1~40 ng/ml范围内线性关系良好(相关系数r=0。9999),平均回收率为114。0%(RSD=8。7%),方法重复性及精密度均良好。结论 该方法操作简单,可实现对消肿止痛酊中马兜铃酸Ⅰ的含量测定。
Content determination of aristolochic acid I in Xiaozhong Zhitong Tincture by LC-MS/MS method
Objective To establish a specific detection method for aristolochic acid I in Xiaozhong Zhitong Tincture,so as to provide theoretical basis for quality control of Xiaozhong Zhitong Tincture.Methods The content determination of aristolochic acid Ⅰ in Xiaozhong Zhitong Tincture was carried out by liquid chromatography-mass spectrometry(LC-MS/MS).Separation was carried out on a Poroshell 120 SB-C18(2.1 mm × 100 mm,2.7 μ m)column,gradient elution was carried out with 0.1%formic acid solution(containing 5 mmol/L ammonium formate)-acetonitrile as the mobile phase,the column temperature was 30 ℃,and the flow rate was 0.3 ml/min.In the positive ion mode of electrospray ionization,multiple reaction monitoring was carried out,and external standard method was used for quantification.Results The linear relationship of aristolochic acid I was good in the range of 0.1-40 ng/ml(correlation coefficient r=0.9999),the average recovery rate was 114.0%(RSSD=8.7%),and the repeatability and precision of the method were both good.Conclusion The method is simple and can be used to carry out the content determination of aristolochic acid I in Xiaozhong Zhitong Tincture.

Liquid chromatography-mass spectrometryXiaozhong Zhitong TinctureAristolochic acid ⅠContent determination

程庆兵、汪海宣、郑正、杨彬、袁杰、王玮

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合肥市食品药品检验中心,安徽 合肥 230071

安徽省食品药品检验研究院,安徽 合肥 230051

液相色谱-质谱联用法 消肿止痛酊 马兜铃酸Ⅰ 含量测定

2024

中国医药科学
海峡两岸医药卫生交流协会 二十一世纪联合创新(北京)医药科学研究院

中国医药科学

影响因子:1.083
ISSN:2095-0616
年,卷(期):2024.14(21)