食品科学 ›› 2017, Vol. 38 ›› Issue (24): 265-271.doi: 10.7506/spkx1002-6630-201724043

• 安全检测 • 上一篇    下一篇

固相萃取-超高效液相色谱-串联质谱法同时测定酸奶中55 种塑料添加剂

薄海波,星玉秀,吉生军,王静莹,杨娟   

  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)
  • 出版日期:2017-12-25 发布日期:2017-12-07
  • 基金资助:
    青海省应用基础研究项目(2014-ZJ-722)

Simultaneous Determination of 55 Plastic Additives Migrating from Plastic Containers to Yogurt by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

BO Haibo, XING Yuxiu, JI Shengjun, WANG Jingying, YANG Juan   

  1. (1. College of Chemistry and Chemical Engineering, Qinghai Normal University, Xining 810008, China;2. Security Department of Criminal Science and Technology, Qinghai Public Security Bureau, Xining 810000, China)
  • Online:2017-12-25 Published:2017-12-07

摘要: 建立高通量的超高效液相色谱-串联质谱检测方法,同时测定酸奶中55?种塑料添加剂,包括多种类的增塑剂、抗氧化剂、紫外线吸收剂、表面活性剂、阻燃剂、着色剂和荧光增白剂等多个类别的化合物。用乙腈提取酸奶样品中的塑料添加剂,HLB固相萃取净化;ACQUITY?UPLC?BEH?C18色谱柱,甲醇-0.1%甲酸为流动相;串联质谱以电喷雾离子源正离子模式电离,多反应监测模式下测定55?种化合物;外标法定量。结果表明:55?种塑料添加剂在较宽的质量浓度范围内线性关系良好,相关系数(r2)均大于0.97;3?个添加水平的回收率在62.4%~93.5%之间,精密度为2.4%~13.4%;酸奶中55?种塑料添加剂的最低检出限为0.2~40?μg/kg。测定20?个酸奶样品,共检出23?种塑料添加剂,含量在7.0~39?μg/kg之间。本方法适用于酸奶中不同类别、物理和化学性质差异大的多种类多组分塑料添加剂的定性确证和高灵敏度定量。

关键词: 塑料添加剂, 超高效液相色谱-串联质谱, 高通量检测, 酸奶

Abstract: A method has been developed to determine 55 plastic additives including antioxidants, plasticizers, ultraviolet light absorbers in yogurt by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). Samples were extracted with acetonitrile and the extract was then cleaned up on an HLB SPE column. The UPLC system equipped with a ACQUITY UPLC BEH C18 analytical column (2.1 mm × 50 mm, 1.7 μm) was operated utilizing methanol-0.1% formic acid as the mobile phase in gradient elution mode. Electrospray ionization in positive ion mode (ESI+) with multiple reaction monitoring (MRM) was used, and the analytes were quantified by the external standard method. The calibration curves displayed good linearity in a wide concentration range with a correlation coefficient of over 0.97. The average recoveries from spiked yogurt at three concentrations ranged from 62.4% to 93.5% with relative standard deviations (RSD) varying from 2.4% to 13.4%. The limits of detection (LOD) were 0.2–40 μg/kg. Twenty-three plastic additives at concentrations from 7.0 to 39 μg/kg were detected in 20 samples by the proposed method. This method can simultaneously identify and quantify a wide variety of plastic additive compounds with distinctive physicochemical properties in yogurt with high sensitivity.

Key words: plastic additives, ultra performance liquid chromatography-tandem mass spectrometry, high throughput detection, yogurt

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