GC-MS/MS法测定不同香型白酒中邻苯二甲酸酯类的含量分析

采用气相色谱-三重四极杆串联质谱法（GC-MS/MS）建立了邻苯二甲酸酯（PAEs）的检测方法，并对12种不同香型白酒中的18种PAEs塑化剂的含量进行了测定。结果表明，18种PAEs的分离效果良好，检出限为0.001～0.428 mg/kg，定量限为0.003～1.426 mg/kg。邻苯二甲酸二异壬酯（DINP）的线性范围为0.403～20.150 μg/mL，其余17种PAEs的线性范围为0.020～1.106 μg/mL，相关系数（R2）均＞0.999，精密度试验结果相对标准偏差（RSD）均＜10%，回收率为82.99%～115.25%；白酒样品检出塑化剂的种类主要为邻苯二甲酸二异丁酯（DIBP）、邻苯二甲酸二正丁酯（DBP）及邻苯二甲酸二（2-乙基）己酯（DEHP），含量分别在0.18～1.53 mg/kg、0.27～1.36 mg/kg、0.18～1.86 mg/kg，其中兼香型白酒样品的DBP含量为1.36 mg/kg，超出国标规定限值。在凤香型白酒样品和馥郁香型白酒样品中检出邻苯二甲酸二甲酯（DMP），含量分别为0.53 mg/kg、0.45 mg/kg，在药香型白酒样品中检出邻苯二甲酸二正辛酯（DNOP），含量为1.42 mg/kg，其余均未检出。

Determination of phthalate esters in different flavor Baijiu by GC-MS/MS

The method for phthalate esters (PAEs) detection was established by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS). Subsequently, the content of 18 PAEs plasticizers in 12 different flavor Baijiu (Chinese liquor) was determined. The results showed that the separation of 18 PAEs was good, the detection limit of PAEs was 0.001-0.428 mg/kg, and the quantitative limit was 0.003-1.426 mg/kg. The linear range of diisononyl phthalate (DINP) was 0.403-20.150 μg/ml, and the linear range of other 17 PAEs was 0.020-1.106 μg/ml. The correlation coefficient (R2) was greater than 0.999, the relative standard deviation (RSD) of precision tests results was less than 10%, and the recovery was 82.99%-115.25%. The main types of plasticizers detected in Baijiu samples were diisobutyl phthalate (DIBP), dibutyl phthalate (DBP) and di-2-ethylhexyl phthalate (DEHP), and the contents were 0.18-1.53 mg/kg, 0.27-1.36 mg/kg and 0.18-1.86 mg/kg, respectively. The DBP content in the compound flavor Baijiu sample was 1.36 mg/kg, exceeding the national standard specified limit. The dimethyl phthalate (DMP) was detected in Feng-flavor and fragrance-flavor Baijiu samples, and the contents were 0.53 mg/kg and 0.45 mg/kg, respectively. The di-n-octyl phthalate (DNOP) was detected in medicine-flavor Baijiu sample, and the content was 1.42 mg/kg, other PAEs were not detected.