Zhu Feng, Ji Wenliang, Liu Hualiang, Jia Yanbo, Cai Mei, Zhang Hao
Jiangsu Provincial Center for Disease Prevention and Control, Nanjing 210009, China.
SCIEX, Beijing 100026, China.
Se Pu. 2017 Sep 8;35(9):957-962. doi: 10.3724/SP.J.1123.2017.04036.
A method was developed for the screening and detection of food poisonings by ultra high performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UHPLC-Q-TOF MS). After extracted by acetonitrile and cleaned-up by QuEChERS, the extract was separated on a Waters Acquity UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) with the gradient elution of 0.1% (v/v) formic acid in water and 0.1% (v/v) formic acid in acetonitrile. TOF-MS scan-information dependent acquisition (IDA)-product ion scan was performed in positive electrospray ionization (ESI) mode to acquire high resolution MS and MS/MS spectra in one injection, and rapidly screen 581 target compounds by SCIEX OS software, including 546 pesticides, 24 mycotoxins, 11 rodenticides. The target compounds were qualitatively confirmed by mass accuracy of precursor, isotope distribution of precursor, fragment ions of precursor, and library search. Carbofuran was detected in 9 out of 11 samples with the proposed method. The retention time was further confirmed by the standard of carbofuran. The results showed the retention times were coincident between the samples and reference standard, and the deviations of accurate mass numbers were all less than 3.7×10. The scope of the relationship was good and the correlation coefficient was 0.998. The instrumental limit of detection (=3) was 0.3 μg/kg, and the limit of quantification (=10) was 1 μg/kg. The recoveries at 10, 50, 200 μg/kg levels were 75.6%-95.9%, and the RSDs (=6) were 3.6%-6.9%. The method is rapid, simple, accurate and sensitive. It is suitable for the rapid screening and detection of public safety incidents.
建立了一种超高效液相色谱-四极杆飞行时间质谱联用(UHPLC-Q-TOF MS)筛查和检测食物中毒的方法。样品经乙腈提取、QuEChERS净化后,在Waters Acquity UPLC BEH C18柱(100 mm×2.1 mm,1.7 μm)上,以含0.1%(v/v)甲酸的水溶液和含0.1%(v/v)甲酸的乙腈溶液进行梯度洗脱分离。采用正电喷雾电离(ESI)模式进行TOF-MS扫描信息依赖采集(IDA)-产物离子扫描,一次进样即可获得高分辨率的MS和MS/MS谱图,并通过SCIEX OS软件快速筛查581种目标化合物,包括546种农药、24种霉菌毒素、11种杀鼠剂。通过母离子质量准确度、母离子同位素分布、母离子碎片离子及谱库检索对目标化合物进行定性确证。采用该方法在11份样品中的9份中检测出了克百威。通过克百威标准品进一步确认保留时间。结果表明,样品与对照品的保留时间一致,精确质量数偏差均小于3.7×10。线性关系良好,相关系数为0.998。仪器检出限(=3)为0.3 μg/kg,定量限(=10)为1 μg/kg。在10、50、200 μg/kg添加水平下的回收率为75.6% - 95.9%,相对标准偏差(=6)为3.6% - 6.9%。该方法快速、简便、准确、灵敏,适用于公共安全事件的快速筛查和检测。