顶空气相色谱-质谱联用法同时测定食品用洗涤剂中的三种成分  

Simultaneous determination of three components in food detergents by headspace gas chromatography-mass spectrometry

作　　者：张颍 姚晨之[1] 严方 李晓婷 Ying Zhang;Chenzhi Yao;Fang Yan;Xiaoting Li(China Research Institute of Daily Chemical Industry,Taiyuan,Shanxi 030001,China;Sinolight Daily Chemical Inspection&Certification Co.,Ltd.,Taiyuan,Shanxi 030001,China)

机构地区：[1]中国日用化学工业研究院,山西太原030001 [2]中轻日用化学检验认证有限公司,山西太原030001

出　　处：《日用化学工业（中英文）》2024年第8期1008-1014,共7页China Surfactant Detergent & Cosmetics

基　　金：自然堂研究基金资助项目(自然堂2021)。

摘　　要：建立了顶空气相色谱-质谱联用仪(HS-GC-MS)同时测定食品用洗涤中的甲醛、甲醇和1,4-二噁烷的方法。方法对顶空进样的影响因素进行了单因素方差分析和正交试验,确定最优试验条件;选择强极性色谱柱SH-Rtx-Wax(30 m×0.32 mm×0.25μm)进行分离;采用选择离子扫描(SIM)模式和外标法定量分析。实验结果表明,甲醛、甲醇和1,4-二噁烷分别在8~200,8~200和2~50μg/mL范围内线性关系良好,检出限(LOD)在0.10~0.60μg/mL,定量限(LOQ)在0.29~1.78μg/mL;对实际样品添加低、中、高三个水平进行加标回收和精密度试验,加标回收率在84.0%~101.9%,相对标准偏差(RSD)在0.5%~3.7%。该方法操作简单、灵敏度高、重复性好,能够满足食品用洗涤剂中甲醛、甲醇、1,4-二噁烷同时测定的要求,同时也为我国食品用洗涤剂相关安全指标提供技术依据和参考。A method for simultaneous determination of methanal,methanol and 1,4-dioxane in food detergents by headspace gas chromatographymass spectrometry(HS-GC-MS)was established.The influencing factors of headspace sampling were analyzed by single factor variance analysis and orthogonal test to determine the optimal conditions.A strong polar column SH-Rtx-Wax(30 m×0.32 mm×0.25μm)was selected for separation.Selective ion scanning(SIM)mode and external standard method were used for quantitative analysis.The results show that methanal,methanol and 1,4-dioxane have good linear relationships in the ranges of 8-200μg/mL,8-200μg/mL and 2-50μg/mL,respectively.The limits of detection(LOD)are 0.10-0.60μg/mL,and the limits of quantification(LOQ)are 0.29-1.78μg/mL.The recovery and precision test of the actual samples are carried out at low,medium and high levels.The recovery rate is 84.0%-101.9%and relative standard deviation(RSD)is 0.5%-3.7%.The method is simple,sensitive and reproducible,which can meet the requirements of simultaneous determination of methanal,methanol and 1,4-dioxane in food detergents,and also provide technical basis and reference for the relevant safety indicators of food detergents in China.

关 键 词：甲醛 甲醇 1 4-二噁烷 顶空 气质联用 食品 洗涤剂 

分 类 号：TQ649[化学工程—精细化工]