气相色谱-质谱法快速筛查食物中毒物质克百威

Rapid screening of food poisoning substance carbofuran by gas chromatography-mass spectrometry

目的通过气相色谱-质谱法对急性克百威食物中毒事件进行快速检测。方法17份可疑样品经乙酸乙酯快速萃取,离心后取上清液,Rxi-5ms色谱柱(30 m×0.25 mm,0.25μm)分离,应用全扫描模式(full scan,Scan)和谱库检索定性中毒物质,通过QuEChERS法前处理和选择离子扫描模式(selective ion monitoring,SIM),外标法定量。结果在凉粉残留物、1份洗胃液、1份血液及2份不明白色粉末样品中均检出氨基甲酸酯类农药克百威及其中间体呋喃酚,其他样品均未检出,凉粉残留物中克百威质量浓度为253.0μg/mL,呋喃酚质量浓度为546.6μg/mL。克百威及呋喃酚在0~5.0μg/mL范围内线性关系良好(r>0.999),检出限(limits of detection,LODs)分别为0.0014~0.0344μg/mL、0.0016~0.0217μg/mL,定量限(limits of quantitation,LOQs)分别为0.0048~0.1146μg/mL、0.0053~0.0722μg/mL,相对标准偏差(relative standard deviations,RSDs)分别为4.6%~6.6%、3.5%~7.6%。在0.25、0.50、1.00μg/mL3个浓度水平的平均加标回收率为81.4%~107.1%,RSDs为1.9%~7.6%。结论此方法操作简单、灵敏度高、稳定性好,为急性食物中毒事件提供了快速、高效的检测方法。

Objective To rapidly detect acute carbofuran food poisoning incidents by gas chromatography-mass spectrometry.Methods The 17 samples were extracted by ethyl acetate,supernatant was taken and separated on Rxi-5ms column(30 m×0.25 mm,0.25μm)after centrifugation.The qualitative toxic substances were retrieved by full scan mode(Scan)and spectrum library,and quantified by external standard method by selecting ion monitoring(SIM)and QuEChERS.Results The carbamate pesticides of carbofuran and furanol of its intermediate were detected in residue of cold powder,1 sample of the gastric lavagehe,1 sample of blood and 2 samples of unknown white powders,none of the other samples were detected,the concentration of carbofuran and furanol residues was 253.0μg/mL and 546.6μg/mL,respectively.The linearity of carbofuran and furanol was good(r>0.999)in the range of 0.1–5.0μg/mL.The limits of detection(LODs)were 0.0014–0.0344μg/mL and 0.0016–0.0217μg/mL,respectively,and the limits of quantitation(LOQs)were 0.0048–0.1146μg/mL and 0.0053–0.0722μg/mL,respectively,the relative standard deviations(RSDs)were 4.6%–6.6%and 3.5%–7.6%,respectively.The average recoveries were 81.4%–107.1%and RSDs were 1.9%–7.6%at 3 different levels of spiked concentration of 0.25,0.50,1.00μg/mL.Conclusion This method is easy to operate,highly sensitive,and stable,providing a fast and efficient detection method for acute food poisoning incidents.