双标多测法测定补骨脂中补骨脂苷、异补骨脂苷、补骨脂素、异补骨脂素的含量  

Determination of psoralenoside,isopsoralenoside,psoralen and isopsoralen in Psoralea Fructus by method of two reference substances for determination of multiple components

作　　者：刘军玲 张亚中 程世云 孙磊[2] 魏锋[2] 马双成[2] LIU Jun-ling;ZHANG Ya-zhong;CHENG Shi-yun;SUN Lei;WEI Feng;MA Shuang-cheng(Anhui Institute for Food and Drug Control,Hefei 230051,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]安徽省食品药品检验研究院,合肥230051 [2]中国食品药品检定研究院,北京100050

出　　处：《药物分析杂志》2020年第10期1799-1807,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立双标多测(TRSDMC)法同时测定补骨脂中补骨脂苷、异补骨脂苷、补骨脂素、异补骨脂素的含量,在节约对照品同时,更好地控制该品种质量。方法:采用HPLC法测定,使用C18柱,流动相为0.4%磷酸溶液-甲醇(44∶56),流速1 mL·min-1,柱温35℃,检测波长285 nm,进样量5μL;以补骨脂苷和补骨脂素为对照,使用DRS origin软件进行双标线性校正预测特征峰的保留时间,并通过替代对照品法获得相对校正因子,计算所得结果与外标法进行比较。结果:通过DRS origin软件拟合的标准曲线预测待测化合物准确,并结合校正因子计算所得含量与外标法测定结果比较,绝对偏差均<0.5 mg·g-1,准确度均>95.0%。20批样品中补骨脂苷、异补骨脂苷、补骨脂素、异补骨脂素含量范围分别为5.0~22.6、16.3~3.0、4.6~13.6、1.8~8.1 mg·g-1。结论:双标线性校正预测保留时间与相对保留时间法相比,前者保留时间预测结果准确度高,色谱柱的适用范围广,方法简便、准确且经济实用,为补骨脂多指标含量测定提供了新的思路和方法。Objective:To establish a two reference substances for determination of multiple components(TRSDMC) method for simultaneous determination of the contents of psoralenoside,isopsoralenoside,psoralen, and isopsoralen in Psoralea Fructus,so as to reduce the use of reference standards and better control the quality. Methods:HPLC method was used. The column was C18,the mobile phase was 0.4% phosphoric acid solutionmethanol(44∶56),the flow rate was 1 mL·min-1,the column temperature was 35 ℃,the detection wavelength was 285 nm,and the sample volume was 5 μL. Psoralenoside and psoralen were used as controls,and DRS origin software was used to perform the linear calibration with two reference substances correction to predict the retention time of characteristic peaks,and a relative correction factor was obtained by replacing the reference method,and the results were compared with the external standard method. Results:The standard curve of the analytes predicted by the DRS origin software was accurate,and the contents calculated by combining the correction factors were compared with the result of the external standard method. The absolute deviation was <0.5 mg·g-1,and the accuracy was >95.0%. The content ranges of psoralenoside,isopsoralenoside,psoralen and isopsoralen in 20 samples were 5.0-22.6 mg·g-1,16.3-3.0 mg·g-1,4.6-13.6 mg·g-1 and 1.8-8.1 mg·g-1. Conclusion:Compared with the relative retention time method,the liner calibration with two reference substances method is more accurate in predicting retention time. The scope of the column is wider and the method is simple,accurate and economical. The liner calibration with two reference substances method provides a new attempt for the determination of multiindex content of Psoralea Fructus.

关 键 词：补骨脂 香豆素类成分 补骨脂苷 异补骨脂苷 补骨脂素 异补骨脂素 双标多测法(TRSDMC) 替代对照品法 DRS origin软件 高效液相色谱 

分 类 号：R917[医药卫生—药物分析学]