气相色谱法测定一次性PVC插管增塑剂ATBC在全血中的溶出  

Determination of ATBC releasing into whole blood from disposable PVC cannula by gas chromatography

作　　者：韩玎玎 吴瑕[1] 李伟 王红[1] HAN Ding-ding;WU Xia;LI Wei;WANG Hong(Institute of Blood Transfusion, Chinese Aeademy of Medical Sciences, Peking Union Medieal College, Chengdu 610052, China;Shanghai MieroPort Medical （ Group ）Co., Ltd., 1601 Zhang Dong Rd., ZJ Hi-Teeh Park, Shanghai 201203, China)

机构地区：[1]中国医学科学院北京协和医学院输血研究所,成都610052 [2]上海微创医疗器械(集团)有限公司,上海201203

出　　处：《药物分析杂志》2018年第6期1049-1054,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：中国医学科学院医学与健康科技创新工程资助(项目编号:2017-I2M-3-021)

摘　　要：目的:在临床条件与极限条件下,建立气相色谱法(GC法)测定一次性使用动(静)脉插管增塑剂乙酰柠檬酸三正丁酯(ATBC)在全血中以及乙醇-水(密度0.937 3~0.937 8 g·cm^(-3))中的溶出量,为该产品的安全性评价提供依据。方法:采用正己烷萃取血液样品中的ATBC以及真空干燥法提取乙醇水中的ATBC,以GC法测定ATBC的含量。其中采用气相色谱柱为Hp-5MS(30 m×0.25 m×0.25μm,美国安捷伦),进样量2μL,进样温度250℃,分流比1∶1,载体流速5 mL·min^(-1),升温程序:初始温度75℃,保持1 min,按15℃·min^(-1)速率升至270℃,保持2 min。并对测定方法进行方法学研究。结果:GC方法测定ATBC质量浓度在5.14~102.8μg·mL^(-1)范围内线性关系良好(r=0.999 7),检测限为1.067 ng,仪器精密度RSD<5%;正已烷萃取法的回收率为(75.1±4.10)%,真空干燥萃取法的回收率为(70.5±2.40)%。在临床条件(2 L·min^(-1),循环4h)下,一次性动静脉插管在全血中增塑剂ATBC的溶出量为(26.96±2.18)mg·套^(-1),在乙醇水中的溶出量为(30.94±0.98)mg·套^(-1);在极限条件(6 L·min^(-1),循环4 h)下,一次性动静脉插管在全血中增塑剂ATBC的溶出量为(15.74±2.50)mg·套^(-1),在乙醇水中的溶出量为(25.71±0.30)mg·套^(-1)。结论:本法经方法学验证,可以用于测定ATBC在全血以及乙醇水中的溶出量,并且发现在相同的浸提介质中,浸提介质的循环速度越快,增塑剂ATBC的溶出量越低,同时在相同浸提条件下,增塑剂ATBC在乙醇水(密度0.937 3~0.937 8 g·cm^(-3))中的溶出量高于全血中的ATBC溶出量。Objective：was establish gas chromagraphy（GC）method for determination of acetyl tributyl citrate（ATBC）released from disposable arterial（intravenous）cannula into fresh blood and ethanol/water with density from 0.937 3 to 0.937 8 g·cm～（-3）,and provide a basis for safety evaluation of the kind of products.Methods：ATBC in the whole blood was extracted by n-hexane and ATBC in the ethanol/water was obtained by vacuum drying method,and the quantification of ATBC was achieved by GC.The GC capillary column was an HP-5 MS（30 m×0.25 mm×0.25 μm,Agilent Technologies）,2 μL was injected by needle at injector temperature of 250 ℃ using split model（1∶1）,and the flow rate of carrier gas（high purity nifrogen）for column was 25 mL· min^-1.Temperacture program for column：75℃ for 1 min,at 15℃·min^-1 to 270℃ remaining 2 min.The determination was verified by methodology study.Results：The data on the methodology study of GC was presented that the calibration curves of ATBC had a good linear relationship（r=0.999 7）in the concentration range of 5.14-102.8 μg·mL^-1,the detection limit was 1.067 ng,instrumental precision showed RSD 5%.The recovery rate of n-hexane extraction was（75.1±4.1）% and the recovery rate of vacuum drying method was（70.5±2.4）%.Under the recommended clinical conditions（2 L·min^-1,circulating 4 hours）,the amount of ATBC released into whole blood was（26.96 ±2.18） mg per set and amount into ethanol/water was（30.94±0.98） mg per set;under the limited clinical conditions（6 L·min^-1, circulating 4 hours）,the amount of ATBC released into whole blood was（15.74 ±2.50） mg per set and amount into ethanol/water was（25.71±0.30） mg per set.Conclusion：This method was valid for determination of ATBC released into whole blood and ethanol/water,and it was found that the released amount of ATBC was increasing with decreased circulation velocity by using the same medium,and the ATBC had a higher migration into ethanol water（density from 0.

关 键 词：乙酰柠檬酸三正丁酯(ATBC) 增塑剂 溶出量 全血 乙醇-水 循环速度 气相色谱法 

分 类 号：R917[医药卫生—药物分析学]