风湿二十五味丸中非法添加的松香酸检测  

Determination of Abietic Acid Illegally Added in Fengshi Ershiwuwei Pills

作　　者：卢洋 刘益庆 LU Yang;LIU Yiqing(Lianyungang Inspection Testing Center of Food and Drug,Lianyungang,Jiangsu,China 222006)

机构地区：[1]江苏省连云港市食品药品检验检测中心,江苏连云港222006

出　　处：《中国药业》2021年第20期69-72,共4页China Pharmaceuticals

摘　　要：目的建立检测风湿二十五味丸中非法添加松香酸的方法。方法采用高效液相色谱法对制剂中的松香酸进行定性,色谱柱为Aglient Eclipse Plus C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.1%甲酸-乙腈(28∶72,V/V),流速为1.0 m L/min,检测波长为241 nm,柱温为20℃,进样量为10μL。采用超高效液相色谱-四极杆-飞行时间串联质谱(UPLC-Q-TOF-MS)法对松香酸进行进一步确认,色谱柱为Agilent Poroshell 120 EC-C_(18)柱(50 mm×2.1 mm,2.7μm),流动相为0.1%甲酸-乙腈(28∶72,V/V),流速为0.3 m L/min,检测波长为241 nm,柱温为25℃,进样量为0.5μL;扫描模式为正离子模式(ESI+),毛细管电压为4.0 kV,毛细管出口电压为175 V,干燥气温度为300℃,干燥气流速为8 L/min,雾化器压力为35 psig,碰撞能量为15 eV;扫描范围m/z 100~1000。结果松香酸质量浓度在32.375~518.000μg/m L范围内与峰面积线性关系良好(n=5),精密度、重复性试验的RSD均小于1.0%;平均加样回收率为100.12%,RSD为0.33%(n=9)。样品的一级质谱、二级质谱均与松香酸对照品一致。结论该方法简便、准确、重复性好,可用于风湿二十五味丸中非法添加的松香酸检测。Objective To establish a method for the determination of the abietic acid illegally added in Fengshi Ershiwuwei Pills.Methods The qualitation of abietic acid in the preparation was determined by the high-performance liquid chromatography(HPLC)method,the chromatographic column was Aglient Eclipse Plus C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was 0.1%formic acid-acetonitrile(28∶72,V/V),the flow rate was 1.0 m L/min,the detection wavelength was 241 nm,the column temperature was 20℃,and the injection volume was 10μL.The composition of abietic acid was further confirmed by UPLC-Q-TOF-MS,the chromatographic column was Agilent Poroshell 120 EC-C_(18) column(50 mm×2.1 mm,2.7μm),the mobile phase was 0.1%formic acid-acetonitrile(28∶72,V/V),the flow rate was 0.3 m L/min,the detection wavelength was 241 nm,the column temperature was 25℃,and the injection volume was 0.5μL.The scanning mode was positive-ion ESI mode(ESI+),the capillary voltage was 4.0 k V,the capillary outlet voltage was 175 V,the temperature of dry gas was 300℃,the dry gas flow rate was 8 L/min,the atomizer pressure was 35 psig,the collision energy was 15 eV,and the scanning range was m/z 100-1000.Results The linear range of abietic acid was 32.375-518.000μg/m L(n=5),and the RSDs of precision and repeatability tests were less than 1.0%.The average recovery of abietic acid was 100.12%with the RSD of 0.33%(n=9).The primary and secondary mass spectra of the sample were consistent with those of abietic acid reference.Conclusion The method is simple,accurate and reproducible,which can be used for the determination of abietic acid illegally added in Fengshi Ershiwuwei Pills.

关 键 词：风湿二十五味丸 松香酸 高效液相色谱法 超高效液相色谱-四极杆-飞行时间串联质谱法 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学]