参三七伤药片(胶囊)中11-羰基-β-乙酰乳香酸含量测定及掺假物松香酸的检查  

Determination of acetyl-11-keto-β-boswellic acid and adulterated abietic acid in Shensanqishang Tablets(Capsules)

作　　者：钱明明 刘益庆 杨颖 QIAN Ming-ming;LIU Yi-qing;YANG Ying(LianYungang inspection testing center of food and drug,Lianyungang 222000,China)

机构地区：[1]连云港市食品药品检验检测中心,江苏连云港222000

出　　处：《中国处方药》2021年第12期22-25,共4页Journal of China Prescription Drug

基　　金：江苏省市场监督管理局科技计划项目(KJ196054)。

摘　　要：目的建立HPLC波长切换法同时测定参三七伤药片(胶囊)中11-羰基-β-乙酰乳香酸及掺伪物松香中松香酸的含量。方法采用Aglient Eclipse Plus C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相:0.1%甲酸-乙腈(28∶72);流速:1.0 ml/min;波长切换:0~30 min,241 nm,30~45 min,251 nm;进样量:10μl。同时采用UPLC-MS/MS方法对检出松香酸的样品进行进一步确证。结果松香酸检测限为0.04 mg/g,11-羰基-β-乙酰乳香酸和松香酸分别在2.012~201.2μg/ml(r=0.9999,n=5)和4.272~427.2μg/ml(r=0.9999,n=5)范围内呈良好的线性关系,其平均回收率分别为99.62%和99.71%。结论该方法简便、准确、重复性好,适用于参三七伤药片(胶囊)中11-羰基-β-乙酰乳香酸及掺伪松香中松香酸的检测。Objective To establish HPLC wavelength switching method to determine acetyl-11-keto-β-boswellic acid and adulterated abietic acid in Shensanqishang Tablets(Capsules).Methods Using the column of Aglient Eclipse Plus C_(18)(250 mm×4.6 mm,5μm)with 0.1%formic acid-acetonitrile(28∶72)as the mobile phase,the flow rate was 1.0 ml/min,the detection wavelength of ultraviolet detector was 241 nm within 0~30 min and 251 nm within 30~45 min,and the injection volume was 10μl.Meanwhile,the method of UPLC-MS/MS was also adopted to further confirm the result of detected samples containing abietic acid.Results The limit of detection for abietic acid was 0.04 mg/g.The linear range of acetyl-11-keto-β-boswellic acid was 2.012~201.2μg/ml,r=0.9999(n=5).The average recovery was 99.62%,and the linear range of abietic acid was 4.272~427.2μg/ml,r=0.9999(n=5),the average recovery was 99.71%.Conclusion The method is simple,accurate and reproducible,can be used for the determination of acetyl-11-keto-β-boswel-lic acid and illegal adulteration of abietic acid in Shensanqishang Tablets(Capsules).

关 键 词：参三七伤药片(胶囊) 11-羰基-Β-乙酰乳香酸 松香酸 掺伪 高效液相色谱法 液-质联用法 

分 类 号：R286.0[医药卫生—中药学]