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目的建立超高效液相色谱-飞行时间质谱(UPLC-TOF-MS)快速、准确筛查不明原因化学性食物中毒尿样中的353种有毒有害物质的方法。方法采用尿液加标后直接进样、稀释2倍和稀释4倍进样的方法选择尿液最佳前处理方法,采用UPLC-TOF-MS测定,从200μg/L和1 mg/L 2个加标水平分别考察方法的检出限、基质效应、回收率和精密度。结果尿液中目标物的检出限范围为0.29μg/L~990μg/L,其中86.7%(306种)的目标物LOD<100μg/L,27种药物的检出限>200μg/L。2个加标水平上,绝对回收率为50%~150%的物质分别为81.0%、87.2%,相对标准偏差(RSD)<10%的物质分别占69.7%、89.8%;1 mg/L水平上,RSD<5%的物质占76.7%。结论方法的准确性和精密度良好,说明该方法适用于尿液中多目标物的快速筛查。
OBJECTIVE To establish a rapid and accurate method for the determination of 353 toxic and hazardous substances in unexplained food-poisoning urine samples by ultra performance liquid chromatography-time of flight mass spectrometry (UPLC-TOF-MS). Methods The optimal pretreatment method of urine was selected by direct injection, double-dilution and quadruplicate injections after spiked with urine. The optimal pre-treatment methods were as follows: 200μg / L and 1 mg / L The spike levels were examined for the method detection limits, matrix effects, recovery and precision. Results The detection limit of the target in urine ranged from 0.29μg / L to 990μg / L, of which 86.7% (306 species) had LOD <100μg / L, and 27 kinds of drugs had the detection limit> 200μg / L. At 2 spiked levels, substances with absolute recovery rates of 50% -150% were 81.0% and 87.2%, respectively, and those with relative standard deviations (RSDs) <10% accounted for 69.7% and 89.8%, respectively; On the RSD <5% of the material accounted for 76.7%. Conclusion The accuracy and precision of the method are good, which shows that the method is suitable for the rapid screening of multi-targets in urine.