超高效液相色谱-四极杆飞行时间质谱法用于食物中毒的快速筛查与确证

发布时间：2018-03-09 12:40

本文选题：超高效液相色谱-四极杆飞行时间质谱　切入点：食物中毒　出处：《色谱》2017年09期 　论文类型：期刊论文

【摘要】：建立了一种利用超高效液相色谱-四极杆飞行时间质谱筛查食物中毒的方法。试样用乙腈提取,QuEChERS净化,以0.1%(v/v)甲酸水溶液和0.1%(v/v)甲酸乙腈溶液为流动相进行梯度洗脱,经Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.7μm)分离。采用四极杆飞行时间质谱信息依赖性扫描(information dependent acquisition,IDA)模式进行分析。该模式可以实现一次进样分析同时获得分析物的一级和二级碎片的精确质量质谱图,结合SCIEX OS软件可对581种目标物质进行快速筛查,其中包括546种农药、24种真菌毒素、11种鼠药,以一级离子精确质量数、一级离子同位素丰度比以及二级碎片进行标准质谱库匹配。应用建立的快速筛选确认检测方法对一起突发性食物中毒安全事件样本进行检测,共检测11份样本,其中9份均检测出呋喃丹。进一步以呋喃丹标准品确认保留时间,结果表明,样品与标准品保留时间一致。呋喃丹的精确质量数偏差均小于3.7×10-6,在0.5~500 ng/mL范围内线性关系良好,相关系数为0.998,仪器检出限(S/N=3)为0.3μg/kg,定量限(S/N=10)为1μg/kg,在10、50、200μg/kg 3个添加水平的回收率为75.6%~95.9%,相对标准偏差为3.6%~6.9%(n=6)。该方法快速、简便、准确、灵敏,适用于突发性公共安全事件的快速筛查与检测要求。
[Abstract]:A method for food poisoning screening by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry was established. The sample was purified by acetonitrile extraction QuEChERS and gradient elution was carried out with 0.1 v / v) formic acid aqueous solution and 0.1% v / v) formic acid acetonitrile solution as the mobile phase. Separated by Acquity UPLC BEH C18 column 100mm 脳 2.1mm ~ 1.7 渭 m, and analyzed by four-pole time-of-flight mass spectrometric information dependent scanning information dependent acquisitions-IDA) model, this model can obtain the accurate mass mass spectra of the first and second order fragments of the analyte at the same time by one sample analysis. In combination with SCIEX OS software, 581 target substances can be screened quickly, including 546 pesticides, 24 mycotoxins and 11 rodents, with the accurate mass number of first-order ions. The first-order ion isotope abundance ratio and the secondary fragments were matched by standard mass spectrometry. A sample of a sudden food poisoning safety event was detected by using the established rapid screening confirmation detection method. A total of 11 samples were detected. Furan was detected in 9 of them. The retention time was confirmed by the standard of furan. The results showed that the retention time of the sample was the same as that of the standard. The deviation of accurate mass number of furan was less than 3.7 脳 10 ~ (-6), and the linear relationship was good in the range of 0.5 ~ 500 ng/mL. The correlation coefficient is 0.998, the detection limit is 0.3 渭 g / kg, the quantitative limit is 1 渭 g / kg, the recovery rate is 75.6% and the relative standard deviation is 3.66.9n / kg. The method is rapid, simple, accurate, sensitive and sensitive. Suitable for rapid screening and detection of sudden public safety events.
【作者单位】：江苏省疾病预防控制中心;SCIEX公司;
【基金】：江苏科技厅科技支撑计划项目(BE2010745) 江苏省“十二·五”科教兴卫工程项目(ZX201109)~~
【分类号】：O657.63;R155.5

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