UPLC-MS法测定胸腺肽注射剂中胸腺肽α_1的含量  

UPLC-MS determination of thymosin α_1 in thymopolypeptide injections

作　　者：李勇[1,2,3] 廖海明[2] 范慧红[2] 梁成罡[2] 杨化新[2] 金少鸿[2] 丁丽霞[2] 

机构地区：[1]中国药科大学,南京210009 [2]中国食品药品检定研究院,北京100050 [3]康哲医药研究(深圳)有限公司,深圳518057

出　　处：《药物分析杂志》2013年第5期849-853,共5页Chinese Journal of Pharmaceutical Analysis

基　　金：国家科技重大专项课题--化学新药质量标准研究与评价技术平台(2011ZX09303-001)

摘　　要：目的:建立UPLC-MS法测定胸腺肽注射剂中胸腺肽α1(Tα1)的含量。方法:选用ACQUITY UPLC BEH Shield RP18色谱柱(150 mm×2.1 mm,1.7μm),以0.1%甲酸-水(v/v)为流动相A,0.1%甲酸-25%乙腈(v/v)为流动相B,梯度洗脱,流速0.2 mL.min-1,选用Waters Acquity UPLC-三级串联四极杆色谱质谱联用仪的选择离子监测(SIM)扫描方式进行监测,电喷雾离子源,正离子方式,选择监测离子为m/z 778.5。结果:胸腺肽α1的线性范围为0.05～0.5μg.mL-1(r>0.99),检出限为0.02μg.mL-1,定量限为0.05μg.mL-1;平均加样回收率为102.0%,RSD小于5%;各种贮存条件下注射剂溶液中胸腺肽α1均较稳定。结论:该方法适用于胸腺肽注射剂中胸腺肽α1的测定。Objective： To establish a UPLC - MS method for thymosin α1（Tα1） determination in thymopolypeptide injections. Methods：An ACQUITY UPLC BEH Shield RP18 column（150 mm×2.1 mm,1.7μm） was adopted;The mobile phase A：0. 1% （v/v） formic acid solution,B ：0. 1% （v/v） formic acid in 25% （v/v） acetonitrile solution was applied with gradient elution at flow rate of 0.2 mL·min^-1. Determination was carried out by electros-pray positive ionization mass spectrometry in the selective ion monitoring（SIM） mode. The ion m/z 778.5 was used to quantify thymosin α1. Results：The linearity was ranged from 0.05～0.5μg·mL^-1（r〉0.99） with the LOD0.02μg·mL^-1 and LOQ 0.05μg·mL^-1. The average recovery was 102. 0% in six samples with intra and inter day RSD both below 5%. Thymosin α1 in injection solutions was found to be stable under various storage conditions.Conclusion ：The established method can be used for determination of thymosin α1 in thymopolypeptide injections.

关 键 词：胸腺肽Α1 胸腺肽注射剂 酸性多肽 免疫调节药物 超高压液相色谱-电喷雾四极杆质谱 选择离子监测(SIM) 反相高效液相色潽 

分 类 号：R917[医药卫生—药物分析学]