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《化学分析计量》 2018年第05期
DOI:10.3969/j.issn.1008-6145.2018.05.003
凝胶渗透色谱-气相色谱-串联质谱法 测定牛奶中的两种光引发剂
陶运来,田素润
安徽省食品药品检验研究院,合肥 230051 
Determination of two photoinitiators in milk by gel permeation chromatography-gas chromatography tandem mass spectrometry
TAO Yunlai, TIAN Surun
Anhui Provincial Institute for Food and Drug Test, Hefei 230051, China 
摘要:建立了采用凝胶渗透色谱(GPC)为净化方式的牛奶中外源性光引发剂二苯甲酮(BP)和4-甲基二苯甲酮(MBP)的气相色谱-串联质谱(GC-MS/MS)测定方法。样品采用乙腈超声辅助提取,经环己烷-乙酸乙酯(体积比为1∶1)溶剂转化后用GPC净化,再通过HP-5MS气相色谱柱分离,最后经串联四极杆质谱仪检测器进行定性、定量同时分析。该方法的线性范围为5~100 μg/L,BP和MBP的线性相关系数(r2)分别为0.997 2和0.998 4,方法定量限均为0.025 mg/kg。在空白牛奶样品中加入0.05,0.25,0.50 mg/kg 3个浓度水平的BP和MBP,BP和MBP的平均回收率为74.0%~92.0%,测定结果的相对标准偏差为5.5%~10.9%(n=6)。该方法具有灵敏度高、准确度和精密度好的优点,适合牛奶中BP和MBP两种光引发剂的检测。  
Abstract:A novel analytical method based on gel permeation chromatography(GPC)-gas chromatography tandem mass spectrometry (GC-MS/MS) technique was developed to determinate the contents of two photoinitiators benzophenone(BP) and 4-methylbenzophenone(MBP) in milk. The target compounds were firstly extracted by ultrasound-assisted extraction method using acetonitrile as the extraction solvents, and then purified and enriched by GPC technique. Qualitative and quantitative analyses were carried out for the analytes under tandem mass spectrometry after the chromatographic separation on a HP-5MS capillary chromatographic column. The results showed that the method had a good linear range from 5 to 100 μg/L, and the correlation coefficients (r2) were 0.997 2 and 0.998 4 for BP and MBP, respectively. The limits of quantification were both 0.025 mg/kg. By adding three different concentrations of 0.05, 0.25, 0.50 mg/kg of BP and MBP into the blank milk samples, the recoveries were obtained in the range of 74.0%-92.0% with the relative standard deviations of 5.5%-10.9%(n=6). The method is sensitive, accurate and suitable for the determination of BP and MBP in milk.  
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Keywords:gel permeation chromatography; gas chromatography tandem mass spectrometry; milk; photoinitiator 
基金:上海市科委“长三角科技联合攻关领域”项目(18395810300) 
本文引用格式:
陶运来,田素润.凝胶渗透色谱-气相色谱串联质谱法测定牛奶中的两种光引发剂[J].化学分析计量,2018,27(5):11-15. TAO Y L,TIAN S R. Determination of two photoinitiators in milk by gel permeation chromatography-gas chromatography tandem mass spectrometry[J]. Chemical analysis and meterage,2018,27(5):11-15. 

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