皮革科学与工程 ›› 2022, Vol. 32 ›› Issue (3): 70-73.doi: 10.19677/j.issn.1004-7964.2022.03.0013

• 标准化与检验 • 上一篇    下一篇

鞋类皮革部件中苯二胺类物质的HPLC-MS/MS测定方法

王宁, 章宦胜, 苗洁, 陈海园   

  1. 温州市质量技术检测科学研究院,浙江 温州 325007
  • 收稿日期:2021-11-02 出版日期:2022-06-28 上线日期:2022-05-16
  • 作者简介:王宁(1987-),女,博士,高级工程师,453827165@qq.com,主要从事鞋革检测与标准化研究工作。
  • 基金资助:
    浙江省市场监管系统科研计划项目(20190334)

Determination of Phenylenediamines in Footwear Leather Components by HPLC-MS/MS

WANG Ning, ZHANG Huansheng, MIAO Jie, CHEN Haiyuan   

  1. Wenzhou Technical Testing Research Institute for Quality, Wenzhou 325007, China
  • Received:2021-11-02 Online:2022-06-28 Published:2022-05-16

摘要: 建立了鞋类皮革部件中对苯二胺、邻苯二胺和间苯二胺含量的高效液相色谱-串联质谱(HPLC-MS/MS)测定方法。该法以甲醇为溶剂进行二次超声提取,净化后的提取液进行HPLC-MS/MS测定,外标法定量。试验结果表明:在5~500 μg/L质量浓度范围内,三种苯二胺的线性相关系数均大于0.997,线性关系良好;在该方法的试验条件下,三种苯二胺的检出限为0.02~0.03 mg/kg,平均加标回收率在89%~106%范围内,相对标准偏差在3%~9%之间。该方法可用于鞋类皮革部件中对苯二胺、邻苯二胺和间苯二胺残留量的检测分析。

关键词: 高效液相色谱-串联质谱法, 对苯二胺, 间苯二胺, 邻苯二胺, 鞋类, 皮革

Abstract: A method for determining the content of p-phenylenediamine, o-phenylenediamine and m-phenylenediamine in footwear leather components was established by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method. Ultrasonic treatment was carried out for two times using methanol as solvent. Then the purified extracting solution was analyzed by HPLC-MS/MS and quantified by external standard method. The results showed that the linearly dependent coefficients of 3 kinds of phenylenediamines are all above 0.9997 in the concentration range of 5-500 μg/L, demonstrating good linear relationships. According to the condition of this study, the detection limits of 3 kinds of phenylenediamines are 0.02-0.03 mg/kg, and the average recovery ratios ranged from 89% to 106%, while the relative standard deviations of 3%-9% were obtained. The developed method was applicable for the determination of p-phenylenediamine, o-phenylenediamine and m-phenylenediamine residues in footwear leather components.

Key words: HPLC-MS/MS, p-phenylenediamine, m-phenylenediamine, o-phenylenediamine, footwear, leather

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