双标多测法在党参5个成分含量测定中的应用<sup>*</sup>

任月, 陈晓虎, 李青, 孙磊, 张毅, 马双成

doi:10.16155/j.0254-1793.2022.06.22

药物分析杂志 >

2022 , Vol. 42 >Issue 6: 1087 - 1095

DOI: https://doi.org/10.16155/j.0254-1793.2022.06.22

标准研讨

双标多测法在党参5个成分含量测定中的应用^*

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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,重庆市药物过程与质量控制工程技术研究中心,重庆401121;
3.重庆市药品技术审评认证中心,重庆 401120;
4.中国食品药品检定研究院,北京 100050

第一作者 Tel:13693494351;E-mail: 1102505190@qq.com

^** 张毅 Tel:(023)86072771;E-mail:zhangyi@cqifdc.org.cn
马双成 Tel:(010)67095272;E-mail:masc@nifdc.org.cn

收稿日期: 2021-06-01

网络出版日期: 2024-06-24

基金资助

^* 重庆市自然科学基金项目(cstc2020jcyj-msxmX0293);国家药典委员会标准提高课题(2021Z01)

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Application of TRSDMC method for the determination of 5 components in Codonopsis radix^*

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1. Chengdu Universityof Traditional Chinese Medicine,Chengdu 611137, China;
2. Chongqing Institute for Food ang Drug Control, Chongqing Engineering Research Center for Pharmaceutical Process and Quality Control, Chongqing 401121, China;
3. Chongqing Technical Center for Drug Evaluation & Certification, Chongqing 401120, China;
4. National Institutes for Food and Drug Control, Beijing 100050, China

Received date: 2021-06-01

Online published: 2024-06-24

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摘要

目的: 建立双标多测法同时测定党参中腺苷、色氨酸、紫丁香苷、绿原酸、党参炔苷的含量,探索双标多测法(双标线性校正法用于色谱峰定性以及采用相对校正因子定量)在党参质量评价中应用的准确性和可行性。方法: 采用HPLC法,以乙腈(A)-0.1%磷酸水溶液(B)为流动相,梯度洗脱(0~10 min,3%A→5%A;10~20 min,5%A→15%A;20~30 min,15%→25%;30~50 min,60%A),流速为1 mL·min^-1,检测波长为257,214,218 nm,柱温25 ℃;在19根不同的C₁₈色谱柱上测定党参中5个成分的实际保留时间,计算各成分在各色谱柱保留时间的平均值,得到各成分的标准保留时间,选取腺苷(峰1)和紫丁香苷(峰3)作为双标化合物,使用双标线性校正法准确定位各成分色谱峰,预测成分在未知色谱柱的保留时间并与相对保留时间法进行比较。以中间峰紫丁香苷为参照物,计算其余成分的相对校正因子,对各成分进行定量,将所得结果与外标法进行比较。结果: 双标线性校正法能够准确预测待测化合物在未知色谱柱的保留时间,比相对保留时间法偏差更小,适用性更强;腺苷、色氨酸、绿原酸、党参炔苷相对于紫丁香苷的相对校正因子分别0.315 2、2.265 4、0.595 5、1.4414,RSD 均小于2%;相对校正因子法和常规外标法的定量结果显示二者无显著性差异。结论: 双标多测法同时测定党参5个成分,简便准确且经济实用,可更好地控制该品种质量。

关键词： 党参; 双标多测法; 双标线性校正法; 色谱峰定性; 相对校正因子法; 腺苷; 色氨酸; 紫丁香苷; 绿原酸; 党参炔苷

本文引用格式

任月, 陈晓虎, 李青, 孙磊, 张毅, 马双成 . 双标多测法在党参5个成分含量测定中的应用^*[J]. 药物分析杂志, 2022 , 42(6) : 1087 -1095 . DOI: 10.16155/j.0254-1793.2022.06.22

Abstract

Objective: To establish a two reference substances for determination of multiple components (TRSDMC) method for the simultaneous determination of adenosine, tryptophan, syringin, chlorogenic acid, and codonopsis in Codonopsis radix, and to investigatethe accuracy and feasibility of TRSDMC methodin the quality evaluation of Codonopsis radix, using liner calibration with two reference substances(LCTRS)for chromatographic peak qualitative and relative correction factor quantitative. Methods: HPLC method was used with acetonitrile as mobile phase A and 0.1% phosphoric acid solution as mobile phase B in gradient elution mode(0-10 min, 3%A→5%A; 10-20 min, 5%A→15% A; 20-30 min, 15%→25%; 30-50 min, 60% A). The flow rate was 1 mL·min^-1, the detection wavelengths were257, 214 and 218 nm and the column temperature was 25 ℃. The actual retention time of five components in Codonopsis radix was determined on nineteen different types of C₁₈ chromatographic columns, the average retention time of each componentin each column was calculated to obtain the standard retention time of each component.Both adenosine(peak 1)and syringin(peak 3)were taken as the linear calibration standards. LCTRS was used for accurately locating the peaks of each component, predicting the retention time of the components on the unknown column. The identification results were compared with those obtained from the relative retention time method. At the same time, external standard method was established, using syringin (whose peak was in the middle) as reference substance.And the quantification results were compared. Results: LCTRS could be used for accurate prediction ofthe retention time of the components tested on unknown column, with smaller deviation and stronger applicability than the relative retention time method.The relative correction factors of adenosine, tryptophan, syringin, chlorogenic acid and lobetyolin were 0.315 2, 2.265 4, 0.595 5 and 1.441 4, respectively. With RSD values less than 2%, there was no significant difference between the contents obtained by TRSDMC and external standard method for each component. Conclusion: TRSDMC can simultaneously determine the five components in Codonopsis radix, which is simple, accurate, economical and practicaland can better control the quality of this variety.

Key words： Codonopsis radix; two reference substances for determination of multiple components method(TRSDMC); liner calibration with two reference substances(LCTRS); chromatographic peak identification; relative correction factor; adenosine; tryptophan; syringin; chlorogenic acid; lobetyolin

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