分散固相萃取结合高效液相色谱-串联质谱法检测一次性筷子中5种杀菌剂
Test method of five types of fungicide in disposable chopsticks by dispersed solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)
投稿时间:2023-12-27  修订日期:2024-01-24
DOI:
中文关键词:  杀菌剂  一次性筷子  高效液相色谱-串联质谱法
英文关键词:fungicide  disposable chopsticks  high performance liquid chromatography-tandem mass spectrometry
基金项目:天津市市场监督管理委员会科技项目(2021-W21)
作者单位
胡晓楠 天津市食品安全检测技术研究院 
张瑞华 天津市食品安全检测技术研究院 
郭文丽 天津市食品安全检测技术研究院 
张艾蕾 天津市食品安全检测技术研究院 
徐慧静 天津市食品安全检测技术研究院 
AuthorInstitution
HU Xiao-Nan Tianjin Institute for Food Safety Inspection Technology 
ZHANG Rui-Hua Tianjin Institute for Food Safety Inspection Technology 
GUO Wen-Li Tianjin Institute for Food Safety Inspection Technology 
ZHANG Ai-lei Tianjin Institute for Food Safety Inspection Technology 
XU Hui-Jing Tianjin Institute for Food Safety Inspection Technology 
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中文摘要:
      目的建立分散固相萃取结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)分析一次性筷子中5种杀菌剂的检测方法。方法一次性筷子试样经1%甲酸乙腈振荡提取,高速离心后取上层提取液,用酸性氧化铝粉末净化,经ZORBAX Eclipse Plus C18色谱柱分离后,采用多反应监测(multiple reaction monitoring, MRM)模式进行5种杀菌剂的测定,基质曲线外标法定量。结果5种杀菌剂在1~500 ng/mL范围内呈现良好线性关系,相关系数r2为0.9967~0.9991,方法检出限为为5.0 μg/kg,定量限为10.0 μg/kg。在5.0、10.0和100.0 μg/kg 3个水平加标回收率为85.6%~106.8%,相对标准偏差为7.3%~9.9%(n=6)。结论该方法针对一次性筷子基质,采用酸性氧化铝粉末的净化方式,前处理方法简单、净化效果好,且灵敏度高、准确性好,适用于一次性筷子中常用杀菌剂的检测。
英文摘要:
      Objective To establish a method for determination of five types of fungicide in disposable chopsticks by dispersed solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample of disposable chopsticks is extracted by acetonitrile with 1% formic acid. The supernatant liquid is taken and purified with acidic alumina powder after high-speed centrifugation. Separated by ZORBAX Eclipse Plus C18 chromatographic column, five types of fungicide are finally determined by using multiple reaction monitoring (MRM). The calibration curve is set up by external standard calibration method. Results The linear relationship of five types of fungicide was strong in the range of 1~500 ng/mL. The coefficient of determination, r2, ranged between 0.9967 and 0.9991. The MDL of the method are 5.0 μg/kg and the LOQ are 10.0 μg/kg respectively. The recovery rates ranged between 85.6 and 106.8% with RSDs varying from 7.3 to 9.9% (n=6) at the concentration of 5.0, 10.0 and 100.0 μg/kg. Conclusion Purified with acidic alumina powder, this method has a simple pretreatment technique, good purification effect, high sensitivity and excellent accuracy, which is especially applicable for the determination of common fungicide in disposable chopsticks.
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