气相色谱-质谱联用法快速检测食物中毒 案例中的克百威农药

Rapid detection of carbofuran pesticide in food poisoning by gas chromatography-mass spectrometry

中文关键词:  食物中毒  气相色谱-质谱法  快速检测  克百威

英文关键词:food poisoning  gas chromatography-mass spectrometry  rapid detection  carbofuran

中文摘要:

      目的 通过气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)快速检测食物中毒案例的样品中克百威农药。方法 使用丙酮快速提取样品, 离心后取上清液, 上机待测。运用全扫描方式监测, 通过全扫描提供的质谱图由谱库检索出可疑物质, 再根据保留时间和质谱图中特征离子准确定性。配制标准系列通过选择离子扫描模式监测方式, 外标法定量。结果 在导致食物中毒的现场采集的样品中检出致毒因子杀虫剂农药克百威。配制克百威标准浓度为0.10~2.00 mg/L范围内呈良好的线性关系, 相关系数(r2)=0.9989, 加标回收率为86%~101%, 相对标准偏差(relative standard deviation, RSD)为2.2%~5.8%。样品中克百威的含量最高达到了232 mg/kg。结论 此方法操作简单、易行, 是快速、有效的一种毒物分析方法。

英文摘要:

      Objective To establish a method of rapid detection of carbofuran in case of food poisoning by gas chromatography-mass spectrometry (GC-MS). Methods The sample was quickly extracted with acetone, and the supernatant was taken after centrifugation to be tested on the machine. They were monitored by full scan mode. The suspicious substances were retrieved from the spectral library by the mass spectrogram provided by the full scan, and then qualitatively determined according to the retention time and the characteristic ions in the mass spectrogram. The standard series of preparation was determined by selected ion monitoring with external standard quantitative. Results Carbofuran was detected in samples, which were collected at the site of food poisoning. The correlation coefficient could reach above 0.998 in the concentration range of 0.10-2.00 mg/L. The spiked recoveries were 86%-101%, with the relative standard deviations (RSDs) of 2.2%-5.8%. The content of carbofuran in the sample reached a maximum of 232 mg/kg. Conclusion This method is simple and easy to operate, which is a rapid and effective method for analysis of poisons.