青稞酒中53种塑料添加剂检测研究

The Determination of 53 Kinds of Plastic Additives in Highland Barley Wine

建立超高效液相色谱-串联质谱(ultra-performance liquid chromatography-tandem mass spectrometry,UPLCMS/MS)法同时测定青稞酒中抗氧化剂、增塑剂、紫外线吸收剂、着色剂等多个类别53种塑料添加剂的高通量快速筛查方法。样品用水稀释至酒精度20%左右,乙腈盐析提取;ACQUITY BEH C_(18)柱(50 mm×2.1 mm,1.7μm),甲醇-0.1%甲酸梯度洗脱分离;电喷雾离子源正离子模式电离(ESI+),多反应监测模式(MRM)分析;外标法定量。结果表明:53种塑料添加剂在较宽浓度范围内线性关系良好,相关系数(r^2)均大于0.99,3个添加水平的平均回收率为71.8%~96.3%,精密度(Relative Standard Deviation,RSD)为1.6%~14.7%(n=6)。检出限(Detection Limit,LODs)和定量限(Quantification Limit,LOQs)分别为0.2μg/L^40μg/L和0.6μg/L^133μg/L。测定12批次青稞酒样品,共检出20种塑料添加剂,分属于多个类别的化合物。

A method has been developed to determine 53 kinds of plastic additives including antioxidant,plasticizer,ultraviolet light absorber and so on in highland barley wine by extraction-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Samples were diluted to 20 % alcohol with water,and extracted with acetonitrile and separated with salting out. The analytes were separated on a reversed phase ACQUITY BEH C_(18) column(50 mm×2.1 mm,1.7μm)and eluted gradiently with methanol and 0.1 % formic acid,and multiple reaction monitoring mode(MRM) was used with electrospray ionization in positive ion mode(ESI+). Analytes were quantified using external standard method. The linear calibration curves were obtained in a wide range with the linear relative coefficients(r^2)more than 0.99. Recoveries from 3 spiked levels ranged 71.8 %-96.3 % and the relative standard deviation(Relative Standard Deviation,RSDs)were 1.6 %-14.7 %(n=6). The limits of detection(Detection Limit,LODs)and the limits of quantification(Quantification Limit,LOQs)for the analytes were 0.2 μg/L-40 μg/L and were 0.6 μg/L-133 μg/L,respectively. Twenty kinds of plastic additives are found in 12 highland barley wine samples.