超高效液相色谱-飞行时间质谱法快速筛查尿液中353种有毒有害化合物  

Ultra performance liquid chromatography-time of flight mass spectrometric method for the rapid screening of 353 toxic compounds in urine

作　　者：李敏[1] 郭巧珍[2] 邵兵[2] 张晶[2] 

机构地区：[1]北京市西城区疾病预防控制中心,北京100120 [2]北京市疾病预防控制中心,北京100013

出　　处：《中国卫生检验杂志》2015年第4期463-466,470,共5页Chinese Journal of Health Laboratory Technology

基　　金：食物中毒诊断溯源技术北京市重点实验室开放基金项目(20130501)

摘　　要：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 ultra performance liquid chromatography- flight mass spectrometry（ UPLC- TOF- MS）method for the rapid and accurate screening of 353 toxc ants in urine samples from unexplained chemical food poisoning. Methods After spiked with standards,the urine samples were determined with no dilution,2- fold and 4- fold dilution to select the best urine pre- treatment method using UPLC- TOF- MS. From spiking level of 200 μg / L and 1 mg / L,the detection limit,matrix effects,recovery and precision of the method were investigated,respectively. Results The detection limits of target compounds was in 0. 29 μg / L- 990 μg / L,of which 86. 7%（306 kinds） of the LODs were less than 100 μg / L,the detection limits of 27 kinds of toxicants were greater than 200 μg / L. For the two spiking levels,the target compounds,whose absolute recovery rates were in 50% to 150%,accounted for 81. 0%,87. 2%,respectively. The target compounds,whose relative standard deviation was less than 10%,accounted for 69. 7%,89. 8%,respectively,on the 1 mg / L level,the target compounds,whose RSD was less than 5%,accounted for 76. 7%. Conclusion The accuracy and precision of the method is good,indicating that the method is suitable for rapid screening of multi- targets in urine.

关 键 词：超高效液相色谱-飞行时间质谱 尿液 化学性食物中毒 毒物筛查 

分 类 号：O657.63[理学—分析化学]