高效液相色谱-串联质谱法测定重组胰岛素中的异丙基硫代半乳糖苷  

Determination of isopropyl-β-D-thiogalactopyranoside in recombinant insulin by high performance liquid chromatography-tandem mass spectrometry

作　　者：金磊 王朋 胡骏杰 刘飞 曹婧[4] JIN Lei;WANG Peng;HU Junjie;LIU Fei;CAO Jing(Nanjing Hanxin Pharmaceutical Technology Co.Ltd.,Nanjing 210000,China;State Key Laboratory of Analytical Chemistry for Life Science,School of Chemistry and Chemical Engineering,Nanjing University,Nanjing 210046,China;College of Forensic Medicine and Laboratory Medicine,Jining Medical University,Jining 272067,China;School of Pharmacy,Nanjing University of Chinese Medicine,Nanjing 210023,China)

机构地区：[1]南京汉欣医药科技有限公司,南京210000 [2]南京大学化学化工学院生命分析化学国家重点实验室,南京210046 [3]济宁医学院法医学与医学检验学院,济宁272067 [4]南京中医药大学药学院,南京210023

出　　处：《分析试验室》2023年第2期172-176,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(21904049);山东省自然科学基金(ZR2019BB037)项目资助。

摘　　要：基于高效液相色谱-串联质谱(HPLC-MS/MS)技术,建立了多肽药物重组胰岛素中残留异丙基硫代半乳糖苷(IPTG)的检测方法。采用乙腈从重组胰岛素粗产品/原料药中萃取IPTG,结合亲水作用色谱(HILIC)分离,在质谱多反应监测(MRM)模式下测定。结果表明,IPTG在0.2~100 ng/mL范围内线性关系良好(R^(2)=0.9969),定量限为0.1 ng/mL,检出限为0.025 ng/mL;在重组胰岛素原料药中加标低、中、高浓度IPTG的回收率为103.3%~106.0%,相对标准偏差为0.6%~4.2%。该方法可作为多肽药物中IPTG杂质含量的质量控制方案。Based on the technology of high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),a method was established for the determination of residual isopropyl-β-D-thiogalactopyranoside(IPTG)in recombinant insulin.Acetonitrile was used to extract IPTG from crude product lactive pharmaceutical ingredient of the recombinant insulin.Hydrophilic interaction chromatography(HILIC)combined with the multireaction detection(MRM)mode of mass spectrometry was applied for the determination of IPTG.The results indicated that IPTG showed a good linear relationship in the concentration range of 0.2-100 ng/mL with R^(2)=0.9969.The limit of quantitation was 0.1 ng/mL,while the limit of detection was 0.025 ng/mL.Spiked recoveries of IPTG at low,medium and high concentrations were 103.3%-106.0%,with the relative standard deviations of 0.6%-4.2%.This method can be used to assure quality control of IPTG impurities in peptide drugs.

关 键 词：高效液相色谱-串联质谱 多肽药物 异丙基硫代半乳糖苷 亲水作用色谱 

分 类 号：R917[医药卫生—药物分析学] O657.63[医药卫生—药学]