质量分析

基于HPLC指纹图谱及双标多测法的四妙丸质量评价研究

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  • 1.成都中医药大学药学院,成都 611137;
    2.重庆市食品药品检验检测研究院,重庆 401121;
    3.江西省药品检验检测研究院,南昌 330029;
    4.西南大学药学院,重庆 400715;
    5.中国食品药品检定研究院,北京 100050
第一作者 Tel:15228992954;E-mail:1297005742@qq.com
* Tel:(023)89029056;E-mail:yangrp@cqacmm.com

收稿日期: 2021-06-25

  网络出版日期: 2024-06-24

Quality evaluation of Simiao pills based on fingerprint combined with TRSDMC*

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  • 1. College of Pharmacy, Chengdu University of TCM, Chengdu 611137, China;
    2. Chongqing Institute for Food and Drug Control, Chongqing 401121, China;
    3. Jiangxi Provincial Research Institute for Drug Control, Nanchang 330029, China;
    4. College of Pharmacy, Southwest University, Chongqing 400715, China;
    5. National Institute for Food and Drug Control, Beijing 100050, China

Received date: 2021-06-25

  Online published: 2024-06-24

摘要

目的: 建立四妙丸指纹图谱,并采用化学计量学方法和双标多测法对四妙丸进行质量评价研究。方法: 采用HPLC法,流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),流速为1 mL·min-1,检测波长为327 nm(0~17 min)、284 nm(18~30 min)、340 nm(31~92 min),柱温为30 ℃。建立四妙丸指纹图谱,使用化学计量学分析进行初步质量评价,再测定四妙丸中8个特征峰在12根不同型号的C18色谱柱上的实际保留时间,双标化合物选定为绿原酸(峰4)和小檗碱(峰14),采用双标线性校正(LCTRS)法预测8个特征峰的保留时间,并在1根未知色谱柱上进行方法验证。再以小檗碱为参照峰,计算绿原酸、黄柏碱的相对校正因子,对各成分进行定量,并将所得结果与外标法进行比较。结果: 13批次四妙丸样品选定16个色谱峰作为指纹图谱的共有峰,经化学计量学分析初步评价其质量;进一步选择采用对照品法归属的8个特征色谱峰进行LCTRS法定性分析。结果表明,LCTRS法预测保留时间的正确率更高(100%),其预测保留时间的准确度优于相对保留时间(RRT)法;绿原酸、黄柏碱相对于小檗碱的相对校正因子分别为0.778 2和0.241 5,以相对校正因子法(RCFM)和常规外标法(ESM)的定量结果显示,二者无显著性差异。结论: 双标线性校正法提高了色谱峰预测保留时间的准确度,能较好地应用于四妙丸多成分的含量测定。

本文引用格式

苟桦梅, 张毅, 吴燕红, 杨荣平, 许妍, 孙磊 . 基于HPLC指纹图谱及双标多测法的四妙丸质量评价研究[J]. 药物分析杂志, 2022 , 42(5) : 866 -874 . DOI: 10.16155/j.0254-1793.2022.05.16

Abstract

Objective: To establish the HPLC fingerprint of Simiao pills, and to evaluate the quality of Simiao pills by using chemometrics and two reference substances for determination of multiple components. Methods: The fingerprint of Simiao pills was established by HPLC, with acetonitrile as mobile phase A and 0.1% phosphoric acid aqueous solution as mobile phase B in gradient elution mode. The flow rate was 1 mL·min-1, the detection wavelength were 327 nm(0-17 min), 284 nm(18-30 min) and 340 nm(31-92 min), and the column temperature was 30 ℃. Chemometrics analysis was used for quality evaluation. The actual retention time of eight characteristic peaks in Simiao pills was determined on 12 different types of C18 chromatographic columns. Chlorogenic acid (peak 4) and berberine(peak 14) were selected as the reference substances for the determination. Linear calibration using two reference substances (LCTRS) method was used to accurately identify the eight characteristic chromatographic peaks, and the method could be verified on an unknown chromatographic column. Taking berberine as reference, the contents of chlorogenic acid and phellodendrine were determined, and the results were compared with the external standard method (ESM). Results: Sixteen chromatographic peaks were selected as common peaks in the fingerprints of 13 batches of Simiao pills. Preliminary evaluation of the quality was made by chemometrics evaluation, and the eight characteristic peaks attributed by reference methodwere further selected for LCTRS. The results show that the LCTRS has a higher accuracy (100%) in predicting retention time.And the LCTRS was superior to the relative retention time(RRT) method. The relative correction factors of chlorogenicacid and phellodendrine to berberine were 0.778 2 and 0.241 5, respectively. The results showed that there was no significant difference between the relative correction factor method(RCFM) and the ESM. Conclusion: The method of LCTRS improves the accuracy of the retention time prediction of chromatographic peaks, and can be better used in the determination of the multi-component content of Simiao pills.

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