白酒中邻苯二甲酸酯检测方法的选择和优化  

Selection and Optimization of the Measurement Method of Phthalate Esters in Liquor

作　　者：李春扬[1] 张晓磊[1,2] 饶静[1,2] 周伟[1,2] 尹建军[1,2] 宋全厚[1,2] 

机构地区：[1]中国食品发酵工业研究院,北京100027 [2]国家食品质量监督检验中心,北京100027

出　　处：《酿酒科技》2013年第2期102-106,共5页Liquor-Making Science & Technology

摘　　要：建立了气相色谱-质谱联用技术(GC-MS),同时测定白酒中16种邻苯二甲酸酯类化合物的检测方法。对前处理影响因素进行探讨,并对操作参数进行优化,确立了最佳试验条件。结果表明,采用氮吹去除酒精后用正己烷提取,采用选择离子监测方式(SIM),以碎片的丰度比定性,外标法定量。该方法检出限为0.05 mg/L,在0.2～5.0 mg/L范围内,线性良好(各相关系数r在0.99526～0.99984之间)。在0.3～1.0 mg/L添加浓度范围内,平均回收率在79.5%～114.7%,相对标准偏差为1.9%～9.4%。该方法简便、快速、准确、灵敏度高,适用于白酒中邻苯二甲酸酯类化合物的分析。A method for simultaneous measurement of 16 kinds of phthalate esters in liquor by gas chromatography-mass spectrometer （GC-MS） had been developed. The factors influencing pretreatment were investigated and the operating parameters were optimized to determine the optimal experimantal conditions. Pressured gas blowing concentrator was used to remove alcohol in the sample and phthalate esters were extracted with n-hexane. Selective ion monitor （SIM） was adopted and phthalate esters were identified by the relative abundance of major characteristic ions and the content was determined by external standard method. The detection limit was 0.05 mg/L, while calibration curves showed good linearity in the range of0.2-5.0 mg/L with the correlation coefficient between 0.995 26 and 0.999 84. The average recoveries ranged fi＇om 79.5 % to 114.7 % with the relative standard deviations （RSDs） between 1.9 % and 9.4 % （n=6） at the spiking levels of 0.3 mg/L and 1.0 mg/L. The method had the advantages including simplicity, speediness, precision and high sensitivity and it was suitable for the determination of phthalate esters in liquor.

关 键 词：白酒 邻苯二甲酸酯 气相色谱-质谱 

分 类 号：TS261.7[轻工技术与工程—发酵工程]