QuEChERS提取-气相色谱/质谱联用法测定食物中毒样品中的克百威

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目的建立Qu ECh ERS提取-气相色谱/质谱联用法(Qu ECh ERS-GC/MS)检测引起化学性食物中毒的有毒物质及其含量,为化学食物中毒应急处理提供科学依据。方法食物中毒样品用乙腈提取,Qu ECh ERS试剂盒提取净化后,通过DB-5MS毛细管色谱柱分离,采用EI源全扫描模式对未知化学毒物定性,采用EI源选择离子监测模式,利用外标法进行定量分析。结果通过对样品质谱图谱分析,在2份样品中检出化学毒物为克百威,样品中克百威浓度分别为581.1 mg/kg、412.5 mg/kg。克百威浓度在0.0 mg/L~5.0 mg/L时线性关系良好,线性相关系数为0.999 1,检出限为0.01 mg/kg,定量限为0.03 mg/kg,加标回收率为80%~97%,相对标准偏差(RSD)为1.2%~3.9%。结论Qu ECh ERS提取-气相色谱/质谱联用法测定食物中毒样品中的克百威,该方法灵敏度高,操作简单快速,重现性好,结果准确,为临床医生抢救患者提供治疗依据。 OBJECTIVE: To establish a Qu ECh ERS-GC / MS method for the detection of toxic substances causing chemical food poisoning and their contents by ERAS-GC / MS, and provide a scientific basis for the emergency treatment of chemical food poisoning. Methods Food poisoning samples were extracted with acetonitrile, purified with Qu ECh ERS kit, separated by DB-5MS capillary column, and identified by EI source scanning mode. EI-selective ion monitoring mode was used. Quantitative analysis. Results The chemical toxicant was detected as carbofuran in 2 samples by mass spectrum analysis. The concentrations of carbofuran in the samples were 581.1 mg / kg and 412.5 mg / kg, respectively. The linearity was good with the concentration of carbofuran between 0.0 mg / L and 5.0 mg / L, the linear correlation coefficient was 0.999 1, the limit of detection was 0.01 mg / kg, the limit of quantification was 0.03 mg / kg and the recovery was 80% ~ 97%, the relative standard deviation (RSD) was 1.2% ~ 3.9%. Conclusion Qu ECh ERS extraction - GC / MS method for the determination of carbofuran in food poisoning samples with high sensitivity, simple and rapid operation, good reproducibility and accurate results provide the basis for clinicians to rescue patients.
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