气质联用测定牙膏中9种卤代烷烃类化合物方法的建立  

Determination of 9 halogenated alkanes in toothpaste by GC⁃MS

作　　者：彭谦[1] 林茜 吴琳媖[1] 宣栋樑[1] PENG Qian;LIN Xi;WU Linying;XUAN Dongliang(Jiading District Center for Disease Control and Prevention,Shanghai 201800,China)

机构地区：[1]上海市嘉定区疾病预防控制中心,上海201800

出　　处：《上海预防医学》2023年第9期905-909,共5页Shanghai Journal of Preventive Medicine

基　　金：上海市嘉定区科学技术委员会课题(JDKW-2020-0027)。

摘　　要：【目的】建立牙膏中9种卤代烷烃类化合物的气质联用分析测定方法。【方法】采集市售多个品牌多种型号的牙膏产品为样品,以甲醇溶液为提取液,经过振摇、涡旋、离心后,取上清液经0.45μm微孔滤膜过滤,滤液采用气质联用测定氯甲烷、二氯甲烷、三氯甲烷、1,1,1-三氯乙烷、四氯化碳、1,2-二氯乙烷、1,1,2-三氯乙烷、1,2-二溴乙烷、1,2,3-三氯丙烷等9种卤代烷烃类化合物的含量。【结果】9种卤代烷烃类化合物在0.03~1.00μg·mL^(-1)浓度范围内呈现良好的线性关系,相关系数≥0.998 7,检出限为0.015~0.056 mg·kg(-1),加标回收率为83.2%~108.9%,相对标准偏差(RSD)为2.0%~9.8%。实际样品检测中有5个品牌共6个牙膏样品分别检出1,1,2-三氯乙烷和1,2,3-三氯丙烷。【结论】该方法操作简便,灵敏度、精密度和加标回收率均较好,可用于牙膏中卤代烷烃类化合物的测定。[Objective]To establish a GC-MS method for the detection of 9 halogenated alkanes in toothpastes.[Methods]Various brands of toothpastes on the market were collected as the samples.Methanol was used as the extraction solution.After shaking,vortex and centrifugation,the supernatant was filtered by 0.45μm microporous filter membrane.The content of 9 halogenated alkanes including chloromethane,dichloromethane,chloroform,1,1,1-trichloroethane,carbon tetrachloride,1,2-dichloroethane,1,1,2-trichloroethane,1,2-dibromoethane,1,2,3-trichloropropane in the filtrate were determined by GC-MS.[Results]The 9 halogenated alkanes showed a good linear relationship in the concentration range of 0.03‒1.00μg·mL^(-1).The correlation coefficient was≥0.9987 with the detection limits of 0.015‒0.056 mg·kg−1.The spiked recoveries were 83.2%‒108.9%with the RSD of 2.0%‒9.8%.In the actual sample analysis,1,1,2-trichloroethane and 1,2,3-trichloropropane were respectively detected in 6 toothpaste samples from 5 brands.[Conclusion]The method is simple,sensitive,accurate,and has good spiked recoveries.It can be used for the determination of halogenated alkanes in toothpastes.

关 键 词：卤代烷烃类化合物 牙膏 气质联用 测定 

分 类 号：R115[医药卫生—公共卫生与预防医学]