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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 gas chromatography tandem mass spectrometry (GC-MS / MS) method for the determination of 18 phthalates (PAEs) in liquor. Methods The liquor sample was vortexed for 1 min with 1 ml of n-hexane and ethyl acetate (1: 1 by volume). The extract was dried over anhydrous sodium sulfate and analyzed by GC-MS / MS with multiple reaction monitoring (MRM) Mode determination. Results The linear range of DINP and DIDP was 0.5 ~ 20μg / ml. The other 16 PAEs [dimethyl phthalate (DMP), phthalate Diethyl phthalate (DEP), Diisobutyl phthalate (DIBP), Dibutyl phthalate (DBP), Di (2-methoxyethyl) phthalate (DMEP ), Bis (4-methyl-2-pentyl) phthalate) (BMPP), di (2- ethoxy) ethyl phthalate (DEEP), diamyl phthalate DPP), dihexyl phthalate (DHXP), butyl benzyl phthalate (BBP), di (2-butoxy) ethyl phthalate (DBEP) (DCHP), di (2-ethylhexyl) phthalate (DEHP), diphenyl phthalate (Dph P), di-n-octyl phthalate (DNOP) The linear range of DNP and DINP was 0.02-2.0μg / ml, and the regression equation showed a good linear relationship with r≥0.996 9. The detection limit of the method was 0.001 0 ~ 0.20μg / ml, the limit of quantification was 0.003 3 ~ 0.66μg / ml, the average recovery was 77.8% ~ 118.3%, RSD was 3.3% ~ 14.8%. Conclusion The method is simple, sensitive and suitable for batch determination of PAEs in liquor.