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

Determination of 5 types of fungicides in disposable chopsticks by dispersed solid phase extraction combined with high performance liquid chromatography-tandem mass spectrometry

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

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, 相关系数为0.9967~0.9991, 方法检出限为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 5 types of fungicides 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 was extracted by acetonitrile with 1% formic acid. The supernatant liquid was taken and purified with acidic alumina powder after high-speed centrifugation. Separated by ZORBAX Eclipse Plus C18 chromatographic column, 5 types of fungicides were finally determined by multiple reaction monitoring (MRM) mode. The calibration curve was set up by external standard calibration method. Results The linear relationship of 5 types of fungicides was strong in the range of 1?500 ng/mL. The correlation coefficient was 0.9967?0.9991, the limit of detection of the method was 5.0 μg/kg and the limit of quantitation was 10.0 μg/kg. The recoveries at the levels of 5.0, 10.0 and 100.0 μg/kg were 85.6%?106.8%, and the relative standard deviations ware 7.3%?9.9% (n=6). Conclusion Purified with acidic alumina powder, this method has a simple pretreatment, good purification effect, high sensitivity and excellent accuracy, which is especially applicable for the determination of common fungicides in disposable chopsticks.