白酒中18种邻苯二甲酸酯的气相色谱串联质谱测定法

Determination of 18 phthalate esters in white spirits by gas chromatography tandem mass spectrometry

目的建立白酒中18种邻苯二甲酸酯（PAEs）的气相色谱串联质谱（GC-MS/MS）法。方法将白酒样品用1 ml正己烷和乙酸乙酯（体积比为1∶1）涡旋振荡提取1 min,提取液用无水硫酸钠脱水后,采用GC-MS/MS多反应监测（MRM）模式测定。结果邻苯二甲酸二异壬酯（DINP）和邻苯二甲酸二异葵酯（DIDP）的线性范围为0.5-20μg/ml,其它16种PAEs[邻苯二甲酸二甲酯（DMP）、邻苯二甲酸二乙酯（DEP）、邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二丁酯（DBP）、邻苯二甲酸二（2-甲氧基）乙酯（DMEP）、邻苯二甲酸二（4-甲基-2-戊基）酯）（BMPP）、邻苯二甲酸二（2-乙氧基）乙酯（DEEP）、邻苯二甲酸二戊酯（DPP）、邻苯二甲酸二己酯（DHXP）、邻苯二甲酸丁基苄基酯（BBP）、邻苯二甲酸二（2-丁氧基）乙酯（DBEP）、邻苯二甲酸二环己酯（DCHP）、邻苯二甲酸二（2-乙基）己酯（DEHP）、邻苯二甲酸二苯酯（Dph P）、邻苯二甲酸二正辛酯（DNOP）、邻苯二甲酸二壬酯（DNP）、邻苯二甲酸二异壬酯（DINP）]的线性范围为0.02-2.0μg/ml,所得回归方程均呈较好的线性关系,r≥0.996 9。方法的检出限为0.001 0-0.20μg/ml,定量下限为0.003 3-0.66μg/ml,平均回收率为77.8%-118.3%,RSD为3.3%-14.8%。结论该方法简单、灵敏度高,适用于白酒中PAEs的批量测定。

Objective To establish a method for the determination of 18 phthalate esters（PAEs） in white spirits by gas chromatography tandem mass spectrometry. Methods The samples of white spirits were treated with the mixture of hexane and ethyl acetate（V ∶V = 1 ∶1） by swirling,the supernatant was dried with anhydrous sodium sulfate and analyzed by gas chromatography tandem mass spectrometry with multiple reaction monitoring（MRM）. Results The linear ranges of DINP and DIDP were 0.5-20 μg/ml,and the other 16 PAEs showed good linearity in the range of 0.02-2.0 μg/ml（r≥0.996 9）. The limits of detection were 0.001 0-0.20 μg/ml,the limits of quantification were 0.003 3-0.66 μg/ml. The average recoveries of spiked samples were 77.8%-118.3% with the RSDs of 3.3%-14.8%. Conclusion The method is suitable for the simultaneous determination of 18 PAEs in white spirits with easy operation and high sensitivity.