超高效液相色谱-串联质谱法测定皮革中9种双酚类物质

doi:10.19677/j.issn.1004-7964.2024.03.009

皮革科学与工程 ›› 2024, Vol. 34 ›› Issue (3): 58-65.doi: 10.19677/j.issn.1004-7964.2024.03.009

超高效液相色谱-串联质谱法测定皮革中9种双酚类物质

王宁^*, 周雷, 章宦胜, 胡秀红, 苗洁

温州市质量技术检测科学研究院,浙江温州 325000

收稿日期:2023-12-18 修回日期:2024-01-25 接受日期:2024-01-27 出版日期:2024-06-01 上线日期:2024-04-25
通讯作者: *
作者简介:王宁（1987-）,女,博士,高级工程师,主要研究方向:鞋类、鞋材检测与标准化。E-mail:453827165@qq.com。
基金资助:
浙江省市场监督管理局科研计划项目（ZC2021B067）; 温州市科研项目（S20220028）

Determination of 9 Bisphenols in Leather by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

WANG Ning^*, ZHOU Lei, ZHANG Huansheng, HU Xiuhong, MIAO Jie

Wenzhou Quality and Technology Testing Research Institute, Wenzhou 325000, China

Received:2023-12-18 Revised:2024-01-25 Accepted:2024-01-27 Published:2024-06-01 Online:2024-04-25

摘要/Abstract

摘要： 建立了皮革中9种双酚类物质的超高效液相色谱-串联质谱测定方法。样品用甲醇超声提取,提取液经固相萃取柱净化后浓缩定容、过滤,采用Agilent ZORBAX Eclipse Plus C18色谱柱（100 mm×3.0 mm,3.5 μm）进行分离,水-甲醇流动相梯度洗脱,采用四级杆质谱仪进行多反应监测分析,内标法定量。结果表明,9种双酚类物质在9 min内可完成分离,线性关系良好,相关系数R2均大于0.999 0,检出限为0.8~24 μg/kg,定量限为4.0~80 μg/kg,加标回收率在85.2%~105.6%范围内,精密度为2.6%~10.3%。鞋用皮革样品测定发现,双酚F、双酚S、双酚A、双酚E和双酚AF均有检出,双酚F和双酚S检出率最高。该法操作简单快速、灵敏度高、精密度好,可为皮革及其制品中双酚类物质的风险监测提供技术支持。

关键词: 液相色谱-串联质谱, 皮革, 双酚, 内分泌干扰物

Abstract: A method for simultaneous determination of 9 bisphenols in leather was established by ultra-high performance liquid chromatography-tandem mass spectrometry. The sample was ultrasonically extracted with methanol. The obtained extract was purified by solid phase extraction column and concentrated to constant volume. The filtrated solution was separated by Agilent ZORBAX Eclipse Plus C18 chromatographic column (100 mm×3.0 mm, 3.5 μm), using water-methanol as mobile phases for gradient elution. Multi-reaction monitoring analysis was performed using a quadrupole mass spectrometer, and internal standard method was adopted for quantification. The results showed that the 9 bisphenols could be separated within 9 min, and the good linear relationships were obtained with correlation coefficients R2 all above 0.999 0. The limits of detection and quantification were in the ranges of 0.8-24 μg/kg and 4.0-80 μg/kg, respectively. The average recoveries were 85.2%-105.6% with precisions of 2.6%-10.3%. Bisphenol F, bisphenol S, bisphenol A, bisphenol E and bisphenol AF were detected in the leathers for shoes, with the higher detection rates for bisphenol F and bisphenol S, respectively. With the advantages of convenient operation, high sensitivity and good precision, the method provides a technical support for risk monitoring of bisphenols in leather and leather goods.

Key words: liquid chromatography-tandem mass spectrometry, leather, bisphenols, endocrine disrupting compounds

中图分类号:

TS943.79

王宁, 周雷, 章宦胜, 胡秀红, 苗洁. 超高效液相色谱-串联质谱法测定皮革中9种双酚类物质[J]. 皮革科学与工程, 2024, 34(3): 58-65.

WANG Ning, ZHOU Lei, ZHANG Huansheng, HU Xiuhong, MIAO Jie. Determination of 9 Bisphenols in Leather by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Leather Science and Engineering, 2024, 34(3): 58-65.

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超高效液相色谱-串联质谱法测定皮革中9种双酚类物质

Determination of 9 Bisphenols in Leather by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

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