液液萃取/气相色谱-质谱法测定氟[^(18)F]脱氧葡糖注射液塑料生产组件浸提液中16种邻苯二甲酸酯类增塑剂  

Determination of 16 Phthalate Plasticizers in the Extracts of Plastic Components Used in the Production of Fludeoxyglucose[^(18)F]Injection by Liquid-Liquid Extraction/Gas Chromatography-Mass Spectrometry

作　　者：昝艳楠 张晓芸 商少华 陈宁 丁逸梅[1,2] ZAN Yan-nan;ZHANG Xiao-yun;SHANG Shao-hua;CHEN Ning;DING Yi-mei(School of Pharmacy,Nanjing University of Technology,Nanjing 211816,China;Drug Testing and Packaging Materials Research Center,Jiangsu Pharmaceutical Research Institute Co.,Ltd.,Nanjing 210009,China)

机构地区：[1]南京工业大学药学院,江苏南京211816 [2]江苏药物研究所有限公司药品检测与包材研究中心,江苏南京210009

出　　处：《分析测试学报》2023年第3期357-362,共6页Journal of Instrumental Analysis

摘　　要：建立了基于液液萃取(LLE)/气相色谱-质谱(GC-MS)检测氟[^(18)F]脱氧葡糖注射液塑料生产组件浸提液中16种邻苯二甲酸酯类(PAEs)增塑剂的方法。根据生产工艺,采用含5%乙醇、5%乙腈的混合溶液作为模拟溶剂,在40℃条件下进行模拟浸提。采用Thermo TG-5 SIL MS色谱柱分离,选择离子扫描模式(SIM)进行分析。通过对仪器条件与萃取条件进行优化,确定最佳前处理方法和仪器条件。在优化实验条件下,16种PAEs在50~500 ng/mL范围内与峰面积呈良好的线性关系,相关系数(r)均不小于0.9906,检出限(LOD)和定量下限(LOQ)分别为10、30 ng/mL。以二氯甲烷为萃取溶剂时,平均回收率为83.0%~114%,相对标准偏差(RSD,n=6)为1.9%~4.2%。采用该方法对浸提液进行测定,16种PAEs均未超过分析评价阈值(AET)。该法操作简便,专属性强,可用于氟[^(18)F]脱氧葡糖注射液塑料生产组件的相容性研究。A method based on liquid-liquid extraction(LLE)/gas chromatography-mass spectrometry(GC-MS)was developed for the determination of 16 phthalate plasticizers(PAEs)in the extracts of plastic components used in the production of fludeoxyglucose[^(18)F]injection.According to the production process,the simulated solvent for extraction experiments was a mixture of 5%ethanol and 5%acetonitrile,and the extraction temperature was simulated at 40℃.The extracts were separated on a Thermo TG-5 SIL MS column,and analyzed in selected ion scanning mode(SIM).The instrument conditions and the extraction conditions were optimized to determine the most suitable pre-treatment method and instrument conditions.Under the optimized experimental conditions,the peak areas of 16 PAEs were linearly correlated in the range of 50-500 ng/mL,with correlation coefficients(r)not less than 0.9906.The limits of detection(LODs)and limits of quantitation(LOQs)were 10 ng/mL and 30 ng/mL,respectively.The average recoveries ranged from 83.0%to 114%with relative standard deviations(RSDs,n=6)of 1.9%-4.2%when dichloromethane was used as the extraction solvent.16 PAEs did not exceed the analytical evaluation threshold(AET)when the extracts were determined by this method.The method is simple and specific,and it could be used to study the compatibility of plastic production components for fludeoxyglucose[^(18)F]injection.

关 键 词：气相色谱-质谱法 液液萃取 增塑剂 氟[^(18)F]脱氧葡糖注射液 塑料组件 

分 类 号：O657.7[理学—分析化学] TS206.4[理学—化学]