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双标线性校正法用于盐沙苑子配方颗粒多组分定性分析

Qualitative determination of multiple components in salted Astragali Complanati Semen dispensing granules by linear calibration using two reference substances
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摘要 目的:建立HPLC-MS法对盐沙苑子配方颗粒中化合物A、杨梅素-3-O-β-D-葡萄糖苷、化合物B、沙苑子苷B、沙苑子苷A进行定性分析,考察双标线性校正(LCTRC)法预测保留时间的可行性,并对LCTRC法和相对保留时间(RRT)法2种替代对照品定性方法进行比较。方法:采用HPLC-MS法,以乙腈为流动相A,以0.1%甲酸水溶液为流动相B,梯度洗脱(0~5 min, 10%A→15%A;5~15 min, 15%A;15~45 min, 15%A→25%A;45~65 min, 25%A→45%A),流速为1.0 mL·min^(-1),柱温为35℃,检测波长为266 nm。通过对照品保留时间及样品的紫外光谱、质谱数据进行样品色谱峰定位,在18根不同品牌或型号的C_(18)色谱柱上,测定盐沙苑子配方颗粒中5个成分的实际保留时间,计算标准保留时间(SRT),以化合物A和沙苑子苷A为双标化合物,使用LCTRC法预测保留时间,并在另外3根C_(18)色谱柱上进行方法验证。同时以中间峰化合物B为参照物,使用RRT法预测保留时间。结果:建立了LCTRC法对化合物A、杨梅素-3-O-β-D-葡萄糖苷、化合物B、沙苑子苷B、沙苑子苷A进行定性分析,5个成分在17根色谱柱上的SRT分别为14.433、19.556、34.071、37.662、39.643 min,线性关系良好(r>0.995)。与RRT法相比,LCTRC法预测保留时间的准确度更高,色谱柱适用范围更广。结论:作为一种新的替代对照品定性方法,LCTRC法能较好地辅助色谱峰定性,值得应用和推广。 Objective:To establish an HPLC-MS method for qualitative determination of compound A,myricetin-3-O-β-D-glucoside,compound B,complanatoside B and complanatoside A in salted Astragali Complanati Semen dispensing granules,in order to detect the feasibility of linear calibration with two reference substances(LCTRC).And the two alternative qualitative methods of reference were compared between LCTRC and the relative retention time method(RRT).Methods:HPLC-MS method was adopted,the mobile phase consisted of acetonitrile(A)-0.2%phosphoric acid aqueous solution(B)with gradient elution(0-5 min,10%A→15%A;5-15 min,15%A;15-45 min,15%A→25%A;45-65 min,25%A→45%A)at a flow rate of 1.0 mL·min^(-1).The column temperature was 35℃and the detection wavelength was 266 nm.The retention time of the 5 components in salted Astragali Complanati Semen dispensing granules were determined on 18 C_(18)columns of different brands or types.The chromatographic peak was identified by retention time of reference and UV spectral and mass spectrum data of sample.The standard retention time(SRT)was calculated.Both compound A and complanatoside A were taken as the two reference substances to forecast the retention time of the other three components by LCTRC.Another 3 C_(18)column was used for methodology validation.Compound B was used as the reference substance to forecast the retention time of the other 4 components by RRT.Results:Compound A,myricetin-3-O-β-D-glucoside,compound B,complanatoside B and complanatoside A were qualitatively analyzed by LCTRC.The retention time of the 5 components on 17 chromatographic columns had good linear relationship(r>0.995),and the SRT of them was 14.433,19.556,34.071,37.662,39.643 min respectively.LCTRC was more accurate and suitable for more chromatographic columns than RRT.Conclusion:As a new alternative reference method,LCTRC can be used to assist the chromatographic peak identification,worthy of application and promotion.
作者 栾永福 刘洪超 解盈盈 许丽丽 郭东晓 马双成 孙磊 林永强 汪冰 LUAN Yong-fu;LIU Hong-chao;XIE Ying-ying;XU Li-li;GUO Dong-xiao;MA Shuang-cheng;SUN Lei;LIN Yong-qiang;WANG Bing(Shandong Institute for Food and Drug Control,NMPA Key Laboratory for Quality Evaluation of Gelatin Products,Shandong Engineering Research Center for TCM Standard Innovation and Quality Evaluation,Shandong Engineering Research Center for Generic Technologies of TCM Dispensing Granules,Jinan 250101,China;National Institutes for Food and Drug Control,Beijing 100050,China)
出处 《药物分析杂志》 CAS CSCD 北大核心 2023年第11期1876-1883,共8页 Chinese Journal of Pharmaceutical Analysis
基金 山东省重点研发计划重大科技创新工程项目(2021CXGC010511) 山东省重点研发计划项目(2020RKB24001) 山东省人文社会科学课题(2021-YYGL-44) 泉城产业领军人才支持计划创新团队项目(MRJT2105)。
关键词 盐沙苑子配方颗粒 高效液相色谱质谱联用 双标线性校正法 相对保留时间法 标准保留时间 色谱峰定性 salted Astragali Complanati Semen dispensing granules HPLC-MS linear calibration with two reference substances(LCTRC) relative retention time chromatographic peak identification standard retention time
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