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食品研究与开发:2016,37(6):150-153
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甜菊糖中18种邻苯二甲酸酯的气相色谱质谱法测定
任民红1,符珍2,左海根1,郭平1,*
(1.江西出入境检验检验局综合技术中心,江西 南昌 330038; 2.南昌大学 食品科学与技术国家重点实验室, 江西 南昌 330047)
Determination of 18 Phthalate Acid Esters in Stevioside by GC-MS
REN Min-hong1, FU Zhen2, ZUO Hai-gen1, GUO Ping1,*
(1.Comprehensive Technology Center of Jiangxi Entry-Exit Inspection and Quarantine Bureau of China Nanchang 330038, Jiangxi,China; 2.State Key Lab of Food Science &Technology,Nanchang University,Nanchang 330047, Jiangxi,China)
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投稿时间:2014-11-13    
中文摘要: 建立甜菊糖中 18 种邻苯二甲酸酯的气相色谱质谱(GC-MS)检测方法。甜菊糖样品加水溶解后经正己烷提取, 采用 GC-MS 测定,外标法定量,线性良好,相关系数大于 0.995,16 种邻苯二甲酸酯的线性范围为 0.02 mg/L~2.0 mg/L 定 量限为 0.05 mg/kg,2 种线性范围为 0.2 mg/L~20 mg/L,定量限为 0.5 mg/kg,样品加标回收率为 76.2 %~116.9 %,相对标准 偏差为 4.2 %~14.3 %,该方法简单、快速、稳定。对 102 个甜菊糖样品进行检测,检出率为 23.5 %,邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基)己酯(DEHP)存在超标的情况。
Abstract:A method was developed for the determination of 18 phthalate acid esters in stevioside by Gas chro- matography-mass spectrometry(GC-MS). The residues in stevioside were extracted by hexane after dissolved in water,and then analyzed by using GC-MS with external standard method. The calibration curve showed a good linearity with the correlation coefficient r2>0.995. The linear range of 16 phthalate acid esters were between 0.02 mg/L and 2.0 mg/L, the quantification(LOQ) limits were 0.05 mg/kg. The linear range of 2 phthalate acid esters were between 0.2 mg/L and 20.0 mg/L, the quantification (LOQ) limits were 0.5 mg/kg. The recoveries were ranged from 76.2 % to 116.9 % with the relative standard deviation(RSDs) of 4.2 %-14.3 % in stevioside. The method was effective and stable. Using the method to detect phthalate acid esters in 102 stevioside sample, the positive rate was 23.5 %, and the contents of dibutyl phthalate, diethylhexyl phthalate were above the limi- tation.
文章编号:201606035     中图分类号:    文献标志码:A
基金项目:国家质检总局课题项目(项目编号:2013IK166)
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