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通过优化前处理条件和仪器条件，建立了一种超声提取技术结合超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定食品包装用胶粘剂中双酚A、烷基酚和烷基酚聚氧乙烯醚三类环境激素的方法。样品经水分散后采用甲醇超声提取，以甲醇-水为流动相，采用XDB-C18柱进行分离，在多反应监测(MRM)模式下测定，外标法定量。考察了标准储备溶液和提取溶液的稳定性，并组织多家实验室进行共同实验。结果表明:所有目标物在20～500 ng/m L浓度范围内标准工作曲线线性关系良好(R2>0.999)，检出限(LOD)为0.20～0.70 mg/kg，定量限(LOQ)为0.68～2.33 mg/kg，平均回收率在88.4%～102.0%之间，日内相对标准偏差<6.0%，日间相对标准偏差<8.0%，方法的重复性限和再现性限分别在0.15～1.68和0.30～1.78范围内。该方法准确度高、精密度好，具有良好的重复性和再现性，操作简便，便于实验室日常大量样品的检测，适用于食品包装用胶粘剂中双酚A、烷基酚和烷基酚聚氧乙烯醚三类环境激素的快速、准确检测。
Abstract：A method was established for the simultaneous determination of three environmental hormones,viz.,bisphenol A,alkylphenols,and alkylphenol ethoxylates,in adhesives used for food packaging through ultrasonic extraction coupled with ultraperformance liquid chromatography-tandem mass spectrometry( UPLC-MS/MS) by optimizing the sample pretreatment and instrumental parameters.The analytical samples were dispersed in water and then extracted by ultrasonic treatment with methanol.Chromatographic separation was performed on an XDB-C18column using methanol-water as the mobile phase. Detection was performed in the multiple reaction monitoring( MRM) mode,and quantification was achieved using an external standard method.The stabilities of both standard stock solutions and extracted sample solutions were investigated,and collaborative tests were conducted in multiple laboratories.The results revealed that all the target analytes exhibited good linear relationships within the concentration range of 20 ～ 500 ng/m L( R2> 0. 999). The limit of detection( LOD) ranged from 0. 20 to 0. 70 mg/kg,and the limit of quantification( LOQ) ranged from 0. 68 to 2. 33 mg/kg.The average recovery ranged from 88. 4% to 102. 0%.The intraand inter-day relative standard deviations( RSDs) were less than 6. 0% and 8. 0%,respectively. The repeatability and reproducibility limits of the method were 0. 15 ～ 1. 68 and 0. 30 ～ 1. 78,respectively.The method developed in this study features high accuracy,satisfactory precision,excellent repeatability and reproducibility,and simple operation.Thus,it is suitable for routine high-throughput analysis in testing laboratories and can be applied in the rapid and accurate determination of three environmental hormones,viz.,bisphenol A,alkylphenols,and alkylphenol ethoxylates,in food packaging adhesives.
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基本信息:
DOI：10.13822/j.cnki.hxsj.2026.0119
中图分类号:O657.63;TS206.4
引用信息:
[1]艾丹,韩路,何静宇,等.液相色谱-串联质谱法测定胶粘剂中常见环境激素[J].化学试剂,2026,48(08):64-71.DOI:10.13822/j.cnki.hxsj.2026.0119.
基金信息:
河南中烟工业有限责任公司科技项目(PW2025005)
2026-05-22
2026
2026-07-14
2026-07-23
2026
1
2026-07-27
2026-07-27
2026-07-27