气相色谱法测定吸附破伤风疫苗中17种邻苯二甲酸酯类增塑剂  

Determination of 17 phthalate plasticizers in adsorbed tetanus vaccine by gas chromatography

作　　者：高彦 鹿泽华 职启航 田文帝 王力 申志强 王斌 GAO Yan;LU Ze-hua;ZHI Qi-hang;TIAN Wen-di;WANG Li;SHEN Zhi-qiang;WANG Bin(Henan Shengming Biotechnology Research Co.,Ltd,Xinxiang 453000,China;Hualan Genetic Engineering Co.,Ltd,Xinxiang 453000,China)

机构地区：[1]晟明生物技术研究院有限公司,新乡453000 [2]华兰基因工程有限公司,新乡453000

出　　处：《药物分析杂志》2023年第3期463-471,共9页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:基于气相色谱法,建立了对吸附破伤风疫苗中17种邻苯二甲酸酯类增塑剂含量测定方法。方法:采用乙腈沉淀蛋白,氯化钠盐析分层,上清液转移、定容后经气相色谱分析,外标法定量。色谱参数:采用Agilent HP-5(30 m×0.32 mm×0.25μm)毛细管柱;升温程序:初始温度为50℃,保持1 min,以20℃·min^(-1)的速率升温至230℃,保持3 min,再以5℃·min^(-1)的速率升温至300℃,保持5 min;色谱柱流量:1 mL·min^(-1);检测器温度:280℃;进样口温度:250℃;载气:氮气,线速度:19.148 cm·s^(-1);进样量:1μL,分流模式:不分流,进样方式:自动进样。结果:17种增塑剂在0.5~20μg·mL^(-1)范围内线性关系良好(r≥0.99)。在15、10、5μg·mL^(-1)3个浓度水平下,加标回收率在83.6%~111.2%之间,RSD为0.39%~3.9%。采用该方法检测5批次吸附破伤风疫苗,药品中均未有增塑剂检出。结论:该方法专属性好,准确度与精密度高,溶液稳定性好,方法耐用性高,能够用于吸附破伤风疫苗药品中增塑剂的含量测定。Objective:To establish a GC-FID method to determine the content of 17 phthalic ester plasticizers in adsorbed tetanus vaccine.Methods:The protein was precipitated with acetonitrile,and the layers were separated by salting out with sodium chloride.The supernatant was transferred and analyzed by GC-FID with external standard method.Agilent HP-5(30 m×0.32 mm×0.25μm)capillary column was adopted.The temperature program:Initial temperature of 50℃was maintained for 1 min,then was increased to 230℃at the rate of 20℃·min^(-1) and was maintained for 3 min.The temperature was increased to 300℃at a rate of 5℃·min^(-1) and maintained for 5 minutes.Column flow rate was 1 mL·min^(-1).The temperatures of detector and inlet were 280℃and 250℃respectively.The linear velocity of the carrier gas(nitrogen)was set to 19.148 cm·s^(-1).The injection volume was 1μL and the split mode was splitless.The sampling mode:automatic injection.Results:The 17 plasticizers showed good linear relationship in the range of 0.5-20μg·mL^(-1) with a correlation coefficient more than 0.99.At three different concentrations(15,10,5μg·mL^(-1))of spiked samples,the re-covery rates of 17 plasticizers ranged from 83.6%to 111.2%,with RSD between 0.39%and 3.9%.No plasti-cizers were detected in 5 batches of adsorbed tetanus vaccine by this method.Conclusion:The method has good specificity,high accuracy and precision,good solution stability,and high durability.It can be used to determine contents of plasticizers in adsorbed tetanus vaccine drugs.

关 键 词：吸附破伤风疫苗 邻苯二甲酸酯增塑剂 气相色谱 包材相容性 含量测定 

分 类 号：R917[医药卫生—药物分析学]