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食品研究与开发:2018,39(1):106-112
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青稞酒中53种塑料添加剂检测研究
吉生军1,星玉秀2,王静莹1,杨娟1,薄海波1,*
(1.青海师范大学化学化工学院,青海西宁810008;2.青海省公安厅刑事科学技术研究管理中心,青海西宁810000)
The Determination of 53 Kinds of Plastic Additives in Highland Barley Wine
JI Sheng-jun1,XING Yu-xiu2,WANG Jing-ying1,YANG Juan1,BO Hai-bo1,*
(1.College of Chemistry and Chemical Engineering,Qinghai Normal University,Xining 810008,Qinghai,China;2.Security Department of Criminal Science and Technology,Qinghai Public Security Bureau,Xining 810000,Qinghai,China)
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投稿时间:2017-06-14    
中文摘要: 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 C18柱(50 mm×2.1 mm,1.7 μm),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(r2)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。
Abstract: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 C18column (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(r2)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 0.2μg/L-40μg/L and were 0.6μg/L-133μg/L,respectively.Twenty kinds of plastic additives are found in 12 highland barley wine samples.
文章编号:201801021     中图分类号:    文献标志码:
基金项目:青海省科技计划项目(2014-ZJ-722)
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