气质联用测定牙膏中<b>9</b>种卤代烷烃类化合物方法的建立

彭谦; 林茜; 吴琳媖; 宣栋樑

doi:10.19428/j.cnki.sjpm.2023.22959

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

摘要

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0.45 μm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0.03~1.00 μg·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。

Abstract:
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 0.45 μm 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 0.03‒1.00 μg·mL^-1. The correlation coefficient was ≥0.998 7 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.

HTML全文

参考文献(15)

施引文献

资源附件(0)