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[1]张慕军,王银松,王洪湘,等.高效液相色谱法测定药物中的哌啶羧酸类化合物[J].天津医科大学学报,2025,31(01):78-84.[doi:10.20135/j.issn.1006-8147.2025.01.0078]
　ZHANG Mujun,WANG Yinsong,WANG Hongxiang,et al.Determination of pipecolic acids and their derivatives in drug substance by High Performance Liquid Chromatography[J].Journal of Tianjin Medical University,2025,31(01):78-84.[doi:10.20135/j.issn.1006-8147.2025.01.0078]
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《天津医科大学学报》[ISSN:1006-8147/CN:12-1259/R]

卷:
31卷
期数:
2025年01期
页码:
78-84
栏目:
技术与方法
出版日期:
2025-01-20

文章信息/Info

Title:
Determination of pipecolic acids and their derivatives in drug substance by High Performance Liquid Chromatography
文章编号:
1006-8147(2025)01-0078-07
作者:
张慕军1; 2; 3; 王银松1; 王洪湘2; 臧慧敏2; 宫雪2
（1.天津医科大学药学院，天津市临床药物关键技术重点实验室，天津 300070；2.天津药物研究院原料药研发中心，天津 300000；3.中国医学科学院药物代谢新技术创新单元，北京 100730）
Author(s):
ZHANG Mujun1; 2; 3; WANG Yinsong1; WANG Hongxiang2;  ZANG Huimin2;  GONG Xue2
（1.School of Pharmacy，Tianjin Medical University，Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics，Tianjin 300070，China；2. Active Pharmaceutical Ingredient Research Center，Tianjin Institute of Pharmaceutical Research， Tianjin 300000，China；3.Research Unit for Drug Metabolism，Chinese Academy of Medical Sciences，Beijing 100730，China）
关键词:
高效液相色谱法; 2; 4-二硝基氟苯; 哌啶羧酸; 柱前衍生
Keywords:
HPLC;  2; 4-dinitrofluorobenzene;  pipecolic acid;  pre-column derivatization
分类号:
R917
DOI:
10.20135/j.issn.1006-8147.2025.01.0078
文献标志码:
A
摘要:
目的：建立高效液相色谱法（HPLC）测定药物中的哌啶羧酸类化合物（PADs）的通用方法。方法：采用2，4-二硝基氟苯（DNFB）作为衍生试剂，使用以十八烷基硅烷键合硅胶为填充剂的色谱柱，0.1%磷酸水和乙腈为流动相进行梯度洗脱，紫外检测器，外标法定量。结果：PADs在不同溶剂中，定量限~3倍限度浓度范围内线性关系均良好，r均大于0.999；定量限回收率均在85%~110%，且相对标准偏差（RSD）均小于4%，50%~200%限度浓度的回收率均在90%~108%，且RSD均小于3%；检测限均小于0.03 μg/mL（相当于供试品溶液浓度的0.007 5%），定量限均小于0.08 μg/mL（相当于供试品溶液浓度的0.020%）。结论：该HPLC方法灵敏度高、通用性强、准确度高，可以作为测定药物中PADs的通用方法。
Abstract:
Objective： To establish a novel High Performance Liquid Chromatography（HPLC） method for the determining pipecolic acids and their derivatives（PADs） in drug substance. Methods： 2，4-dinitrofluorobenzene（DNFB） was used as a derivative reagent， chromatographic column with octadecylsilane bonded silica gel as the filler was used. And water containing 0.1% phosphoric acid-acetonitrile system was utilized as a mobile phase with UV detector， and external standard method was used to quantity. Results： All PADs in different solvents had good linear relationship in between the range of the limit of quantitation（LOQ） to 300% with respect to specification limit， and all the linear correlation coefficients（r） were greater than 0.999. The spiked recoveries of LOQ were all between 85% and 110%， and relative standard deviation（RSDs） were all less than 4%. The spiked recoveries of 50% to 200% with respect to specification limit were all between 90% and 108%， and RSDs were all less than 3%. The limit of detection（LODs） were all less than 0.03 μg/mL（0.007 5% with respect to the concentration of the sample solution）， LOQs were all less than 0.08 μg/mL（0.020% with respect to the concentration of the sample solution）. Conclusion： This HPLC method has high sensitivity， strong universality， and high accuracy， which can be used as a universal method for quantitative determining PADs in drug substance.

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备注/Memo

备注/Memo:
作者简介：张慕军（1983-），男，副研究员，硕士，研究方向：药学；通信作者：王银松，E-mail： wangyinsong@tmu.edu.cn。
更新日期/Last Update: 2025-02-10