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采用改进的液-液萃取提取方法:样品在置于具塞试管中,于80℃水浴敞开加热20 min,用正己烷萃取,微孔膜过滤,建立气相色谱-质谱(GC-MS)法测定黄酒中17种邻苯二甲酸酯类化合物的方法。该方法线性相关系数>0.997,检出限为0.005~0.05 mg/kg之间;在0.1 mg/kg和1.0 mg/kg添加水平时样品加标回收率为74.62%~103.35%,RSD(n=6)为2.36%~8.65%。并运用该方法对市售的黄酒进行了检测。结果表明,在62批陶坛盛装的黄酒样品中,有6批黄酒检出4种邻苯酸二甲酯类化合物,分别是邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸二辛酯(DEHP),它们的含量范围分别是:0.13~0.23 mg/kg、0.04~0.21 mg/kg、0.05~0.10 mg/kg和0.03~0.39 mg/kg。该方法灵敏度高,准确,抗干扰能力强,能同时测定黄酒中包括邻苯二甲酸二异壬酯(DINP)在内的17种邻苯二甲酸酯类化合物的含量。
A modified liquid-liquid extraction method was used. The sample was placed in a plugged test tube, heated in a water bath at 80 ℃ for 20 min, extracted with n-hexane and filtered through a microporous membrane to establish a gas chromatography-mass spectrometry (GC-MS) Method of 17 Phthalates in Rice Wine. The linear correlation coefficient of this method was> 0.997 with the detection limit of 0.005 ~ 0.05 mg / kg. The recoveries of spiked samples were 74.62% ~ 103.35% at 0.1 mg / kg and 1.0 mg / kg, 6) is 2.36% ~ 8.65%. The method was applied to the detection of commercially available rice wine. The results showed that among the 62 batch samples of rice wine, there were 6 batches of yellow rice wine detected four kinds of dimethyl phthalate compounds, namely dimethyl phthalate (DMP), dibutyl phthalate (DBP), DIBP and DEHP in the range of 0.13 ~ 0.23 mg / kg, 0.04 ~ 0.21 mg / kg, 0.05 ~ 0.10 mg / kg and 0.03 ~ 0.39 mg / kg. The method is sensitive, accurate and has good anti-interference ability. It can simultaneously determine the content of 17 kinds of phthalates in rice wine including diisononyl phthalate (DINP).