Prime HLB SPE净化结合高效液相色谱串联质谱法测定羊奶粉中6种消毒剂残留
CSTR:
作者:
作者单位:

作者简介:

邓航(1993-),男,硕士,质量检验工程师,研究方向:食品安全检测,E-mail:975351472@qq.com

通讯作者:

中图分类号:

基金项目:

湖南省产商品质量检验研究院科研资助计划项目(Y2022N11)


Determination of Residues of Six Disinfectants in Goat Milk Powder by Prime HLB SPE Purification Combined with HPLC-MS/MS
Author:
Affiliation:

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    摘要:

    建立了一种高效液相色谱串联质谱法测定羊奶粉中十二烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵、N-十六烷基二甲基苄基氯化铵、十二烷基三甲基溴化铵、二奎基二甲基氯化铵和四丁基硫酸氢铵6种消毒剂的分析方法。样品经热水溶解后,乙腈超声提取并去除蛋白,氯化钠辅助分离,经过Prime HLB固相萃取柱净化后,在Hypersil GOLD C18色谱柱(100 mm×2.1 mm, 2.1 μm)上分离,采用电喷雾离子化(ESI+),多反应监测模式(SRM)进行检测,依据待测样品类型分别采用非脱脂羊奶粉和脱脂羊奶粉空白基质外标法定量。结果显示,6种消毒剂在0.01~5.0 μg/L线性范围内相关系数(R2)均大于0.999。方法检出限(S/N≥3)为0.05 μg/kg,定量限(S/N≥10)为0.10 μg/kg。以羊奶粉作为样品,采用加标回收测得回收率在97.07%~105.6%之间,相对标准偏差(RSD,n=6)在0.987%~4.576%之间,该方法灵敏度高,操作简便,定量准确,可满足羊奶粉中6种消毒剂残留的检测工作要求。

    Abstract:

    A method was developed for the determination of residues of six disinfectants, dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, benzyl dimethyl hexadecyl ammonium chloride, dodecyl trimethyl ammonium bromide, didecyl dimethyl ammonium chloride, and tetra butyl ammonium hydrogen sulfate, in goat milk using HPLC-MS/MS. Each sample was dissolved in hot water, extracted by ultrasonication followed by protein precipitation with acetonitrile, and separated using sodium chloride. Purification was performed using a Prime HLB SPE column before separation on a Hypersil GOLD C18 chromatographic column (100 mm×2.1 mm, 2.1 μm). Detection was conducted using electrospray ionization (ESI+) in selected reaction monitoring mode. Quantification of non-skimmed and skimmed goat milk powder samples was conducted using an external standard method specific to each blanked matrix type. The results demonstrated excellent linearity (correlation coefficients >0.999) within the concentration range of 0.01~5.0 μg/L for all six disinfectants, with detection limits (S/N≥3) and quantitation limits (S/N≥10) determined as 0.05 μg/kg and 0.10 μg/kg, respectively. Spiked recovery tests using goat milk powder samples yielded recoveries ranging from 97.07% to 105.6%, with relative standard deviations (n=6) between 0.987% and 4.576%. This method is highly sensitive, simple, and accurate for quantifying six disinfectant residues in goat milk powder, meeting the requirements for detection.

    参考文献
    相似文献
    引证文献
引用本文

邓航,张可欣,陈少琴,吴社莲,陈思妤,黄潇宁. Prime HLB SPE净化结合高效液相色谱串联质谱法测定羊奶粉中6种消毒剂残留[J].现代食品科技,2025,41(4):349-358.

复制
分享
文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2024-02-21
  • 最后修改日期:
  • 录用日期:
  • 在线发布日期: 2025-05-08
  • 出版日期:
文章二维码