色谱

色谱

• 研究论文 • 上一篇    下一篇

凝胶渗透色谱净化-超高效液相色谱-串联质谱法测定皮革制品中7种尼泊金酯类防腐剂

吴刚1,2*, 赵珊红1, 吴俭俭1, 董锁拽3, 郭方龙1, 王力君1, 叶庆富2   

  1. 1. 浙江省检验检疫科学技术研究院, 浙江 杭州 310015; 2. 浙江大学原子核农业科学研究所, 浙江 杭州 310029; 3. 浙江出入境检验检疫局丝类检测中心, 浙江 杭州 310012
  • 收稿日期:2011-02-18 修回日期:2011-04-07 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 吴刚,博士,高级工程师,主要从事生态纺织品检测与环境毒理学研究. Tel: (0571)28969301
  • 基金资助:

    国家质检总局科研项目(项目编号: 2011IK110)与浙江出入境检验检疫局科研项目(项目编号: ZK200955)

Determination of 7 nipagin ester preservatives in leather by ultra performance liquid chromatography-tandem mass spectrometry coupled with gel permeation chromatographic clean-up

  1. 1. Zhejiang Academy of Science and Technology for Inspection & Quarantine, Hangzhou 310015, China; 2. Institute of Nuclear Agricultural Sciences, Zhejiang University, Hangzhou 310029, China; 3. Silk Testing Center, Zhejiang Entry-Exit Inspection & Quarantine Bureau, Hangzhou 310012, China
  • Received:2011-02-18 Revised:2011-04-07 Online:2011-06-28 Published:2011-07-25
  • Contact: Gang WU

PDF

519

被引次数

25

摘要： 利用超高效液相色谱-串联质谱(UPLC-MS/MS)结合凝胶渗透色谱(GPC)技术,建立了一种快速分离和测定皮革制品中7种尼泊金酯类防腐剂的分析方法。样品经超声提取、浓缩、GPC净化,甲醇-水溶液(1:1, v/v)溶解,采用Acquity UPLCBEH C18柱(50 mm×2.1 mm, 1.7 μm)分离,以甲醇和水为流动相,梯度洗脱,电喷雾负离子模式电离,采用多反应监测模式检测和外标法定量。该方法在0.1～1.0 mg/L范围内线性关系良好(r＞0.99);在添加量为0.5～3.0 mg/kg时,平均回收率为(79.44±5.67)%～(98.07±9.50)%,相对标准偏差(RSD)为4.24%～14.00%;方法的检出限(LOD)为4～12 μg/kg,定量限(LOQ)为13.2～39.6 μg/kg。该方法操作简便、快捷、灵敏、准确,适合皮革中多种尼泊金酯类防腐剂的确证和定量测定。

关键词: 超高效液相色谱－串联质谱, 防腐剂, 尼泊金酯, 皮革

Abstract: A novel method has been developed for the rapid separation and determination of 7 nipagin ester preservatives in leather by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) coupled with gel permeation chromatographic (GPC) clean-up. Nipagin ester preservatives in leather were extracted by ultrasonic extraction with methanol. The extract was dried by a rotavapor and purified by GPC, then redissolved in the solvent of methanol-water (1:1, v/v). The chromatographic analysis was performed on an Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) with a gradient elution of methanol and water as the mobile phases. The analytes were detected by electrospray ionization (ESI) tandem mass spectrometry with multiple reaction monitoring (MRM) in negative ion mode. Good linearity (r＞ 0.99) was observed between 0.1 and 1.0 mg/L for all the analytes. The recoveries and relative standard deviations (RSDs) were checked by spiking samples with the 7 nipagin ester preservatives at the three levels of 0.5, 1.0 and 3.0 mg/kg. The average recoveries of the 7 nipagin ester preservatives were from (79.44±5.67)% to (98.07±9.50)%. The precision values expressed as RSD ranged from 4.24% to 14.00% (n=6). The limits of detection were 4~12 μg/kg and the limits of quantification were 13.2~39.6 μg/kg for the analytes. The method is simple, rapid, sensitive and accurate, and suitable for the quantitative determination and confirmation of 7 nipagin ester preservatives in leather.

Key words: leather, preservatives, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), gel permeation chromatography (GPC), nipagin esters