超高效液相色谱-串联质谱法快速测定食源性中毒患者生物样品中的米酵菌酸  

Determination of bongkrekic acid in biological samples of poisoned patients with foodborne poisoning by UPLC-MS/MS

作　　者：张宏峰[1] 周思 何荣 胡国媛[1] 李泳光 罗晓燕[1] 潘心红[1] 彭荣飞[1] ZHANG Hong-feng;ZHOU Si;HE Rong;HU Guo-yuan;LI Yong-guang;LUO Xiao-yan;PAN Xin-hong;PENG Rong-fei(Guangzhou Center for Disease Control and Prevention,Guangzhou,Guangdong 510440,China)

机构地区：[1]广州市疾病预防控制中心理化检验部,广东510440

出　　处：《现代预防医学》2021年第15期2815-2818,2824,共5页Modern Preventive Medicine

基　　金：广东省医学科学技术研究基金项目(A2020197);广州市卫生健康科技项目(20191A011065,20191A011049)。

摘　　要：目的建立快速测定中毒患者血液、尿液、胃液、血滤废液及血浆置换废液中米酵菌酸的超高效液相色谱-串联质谱测定方法。方法试样经0.1%氨水甲醇-乙腈溶液(80∶20,v/v)涡旋提取、离心、过滤,采用BEH C_(18)柱分离,0.05%甲酸水和甲醇为流动相梯度洗脱,电喷雾离子源负模式(ESI^(-))检测,外标法定量。结果米酵菌酸在0.5~100μg/L浓度范围内线性相关系数为0.9994,方法检出限为0.5μg/L,定量限为1.5μg/L。回收率为74.2%~111.9%,相对标准偏差为0.8%~3.4%(n=6)。结论该方法简单、灵敏、准确,可用于米酵菌酸中毒事件的病因鉴定和治疗效果的快速评估。Objective To develop a rapid determination method for bongkrekic acid in the human blood,urine,gastric juice,waste fluid generated during the hemofiltration and to establish plasmapheres using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Method The sample was vortex extracted with 0.1% ammonia methanol-acetonitrile solution(80∶20,v/v),centrifuged,and filtered.The bongkrekic acid in sample was separated by BEH C_(18) column with 0.05% formic acid water and methanol as mobile phase,detected with a triple quadrupole mass spectrometer,equipped with the electrospray ionization in the negative ion mode,and external standard method for quantification.Results The correlation coefficient of the method in the range of 0.5-100μg/L was greater than 0.9994.The detection limit of the method was 0.5μg/L,and the limit of quantification was 1.5μg/L.Recoveries were in a range of 74.2%-111.9% with the relative standard deviations(RSDs)ranging from 0.8%to 3.4% at the levels of 5.0-50.0μg/L,respectively.Conclusion The method is simple,sensitive,accurate,and can be used for etiological identification and rapid evaluation of therapeutic effect of the patients with bongkrekic acid poisoning.

关 键 词：米酵菌酸 生物样品 超高效液相色谱-串联质谱法 

分 类 号：R115[医药卫生—公共卫生与预防医学]