中国食品卫生杂志2024,Vol.36Issue(6) :688-694.DOI:10.13590/j.cjfh.2024.06.008

超高效液相色谱-质谱法测定被膜剂中烷基苯酚聚氧乙烯醚类

Determination of alkylphenol ethoxylates in coating agent by ultra high performance liquid chromatography-mass spectrometry

范小龙 褚毅宏 吴婉琴 江丰 朱松松 朱正伟 朱晓玲 张亚珍 王福燕
中国食品卫生杂志2024,Vol.36Issue(6) :688-694.DOI:10.13590/j.cjfh.2024.06.008

超高效液相色谱-质谱法测定被膜剂中烷基苯酚聚氧乙烯醚类

Determination of alkylphenol ethoxylates in coating agent by ultra high performance liquid chromatography-mass spectrometry

范小龙 1褚毅宏 2吴婉琴 1江丰 1朱松松 1朱正伟 1朱晓玲 1张亚珍 1王福燕3
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作者信息

  • 1. 湖北省食品质量安全监督检验研究院,湖北武汉 430075;湖北省食品质量安全检测工程技术研究中心,湖北武汉 430075;国家市场监管重点实验室(动物源性食品中重点化学危害物检测技术),湖北武汉 430075
  • 2. 赛默威(湖北)智能科技有限公司,湖北武汉 430075
  • 3. 江汉大学医学部,湖北武汉 430075
  • 折叠

摘要

目的 建立超高效液相色谱-质谱法(UPLC-MS)测定被膜剂中辛基苯酚聚氧乙烯醚(OPEO)和壬基苯酚聚氧乙烯醚(NPEO)的含量.方法 被膜剂样品经水提取,固相萃取柱净化后,采用Thermo Acclaim RSLC 120 C18(2.1 mm×100mm,2.2µm)色谱柱分离,乙腈和0.1%甲酸水为流动相,梯度洗脱,电喷雾正离子模式,选择离子监测模式定量.结果 OPEO和NPEO在0~400 µg/L浓度范围内线性良好(r2>0.996),在0.12、0.24、1.2mg/kg添加水平下的平均回收率为88.5%~96.9%,相对标准偏差为2.9%~7.0%,两种化合物定量限均为0.12 mg/kg.结论 该方法操作简便、快速、准确,其灵敏度、准确度和精密度均适用于被膜剂中烷基苯酚聚氧乙烯醚类的定性分析和定量检测.

Abstract

Objective A method of ultra performance liquid chromatography-mass spectrometry(UPLC-MS)was established for the determination of octylphenol ethoxylates(OPEO)and nonylphenol ethoxylates(NPEO)in coating agent.Methods Samples were extracted with water,and purified by solid phase extraction column.And Thermo Acclaim RSLC 120 C18(2.1 mm×100 mm,2.2 µm)chromatographic column was used for separation.Acetonitrile and 0.1%formic acid water were mobile phase,gradient elution and quantification was performed in SIM mode with positive ion mode of electrospray ionization.Results Octylphenol ethoxylates(OPEO)and nonylphenol ethoxylates(NPEO)were in the range of 0-400 μg/L,and the linear relationships was good(r2>0.996).The recoveries at three spiked levels(0.12,0.24 mg/kg,1.2 mg/kg)were 88.5%-96.9%with the relative standard deviation of 2.9%-7.0%,and the limits of quantitative was 0.12 mg/kg.Conclusion The method was simple,rapid and accurate.Its sensitivity,accuracy and precision were suitable for the quantitative analysis and determination of alkylphenol ethoxylates in coating agent.

关键词

超高效液相色谱-质谱法/被膜剂/烷基苯酚聚氧乙烯醚类

Key words

Ultra high performance liquid chromatography-mass spectrometry/coating agent/alkylphenol ethoxylates

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出版年

2024
中国食品卫生杂志
中国卫生信息与健康医疗大数据学会

中国食品卫生杂志

CSTPCD北大核心
影响因子:1.173
ISSN:1004-8456
参考文献量21
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