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气相色谱串联质谱法测定市售白酒中18种邻苯二甲酸酯类塑化剂

Determination of 18 phthalate plasticizers in liquor by gas chromatography-tandem mass spectrometry

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【作者】 陈俊秀; 马晓年; 张瑞雨; 梁志坚; 梁孟军; 李文廷;

【Author】 CHEN Jun-xiu;MA Xiao-nian;ZHANG Rui-yu;LIANG Zhi-jian;LIANG Meng-jun;LI Wen-ting;Kunming Center for Disease Control and Prevention;

【机构】 云南省昆明市疾病预防控制中心;

【摘要】 为建立气相色谱串联质谱法测定白酒中18种邻苯二甲酸酯类化合物含量,样品经涡旋、离心、正己烷提取等前处理后,采用MEGA-5色谱柱分离、多离子监测扫描模式(MRM),以碎片丰度比定性,外标法定量,测定白酒中的18种邻苯二甲酸酯类化合物含量。结果表明,该方法在给定标准溶液浓度范围内峰面积与浓度呈良好线性关系,相关系数在0.994 0~0.999 8之间,其中邻苯二甲酸二壬酯(DINP)的检出限为3.0 mg/kg,其余17种邻苯二甲酸酯类的检出限为0.1~0.2 mg/kg,平均回收率为70%~130%之间,相对标准偏差均小于10%。对36件样品进行检测,检出1种或几种邻苯二甲酸酯,邻苯二甲酸二正丁酯(DBP)检出率最高,检出率为47.2%。该方法具有灵敏度高、重复性好、检测速度快的优点,可用于白酒中邻苯二甲酸酯类的检测。

【Abstract】 To establish a method for the determination of 18 phthalic acid esters in liquor by gas chromatography-mass spectrometry,the samples were subjected to pretreatment such as vortex,centrifugation and n-hexane extraction,and separated by MEGA-5 chromatographic column. The multiion monitoring scanning mode(MRM)was used to determine the content of 18 phthalate esters in liquor by qualitative analysis of fragment abundance ratio and quantitative analysis by external standard method. The results showed that the linear relationship between peak area and concentration in a given standard solution concentration range was good,and the correlation coefficient was 0.994 0~0.999 8. The detection limit of dinonyl phthalate(DINP)was 3.0 mg/kg,and the detection limits of the other17 phthalate esters were 0.1~0.2 mg/kg. The average recovery was 70%~130%,and the relative standard deviation was less than 10%.Among 36 samples,one or several phthalic acid esters were detected,and the detection rate of di-n-butyl phthalate(DBP)was the highest(47.2%). This method had the advantages of high sensitivity,good repeatability and fast detection speed,which could be used for the detection of phthalate in liquor.

【基金】 昆明市卫生科技人才培养项目暨“十百千”工程培养计划[2019-sw(后备)-50]
  • 【文献出处】 湖北农业科学 ,Hubei Agricultural Sciences , 编辑部邮箱 ,2023年01期
  • 【分类号】O657.63;TS262.3
  • 【下载频次】78
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