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预防医学  2019, Vol. 31 Issue (12): 1205-1209    DOI: 10.19485/j.cnki.issn2096-5087.2019.12.004
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液相色谱-串联质谱法测定食源性中毒患者血浆中米酵菌酸
徐小民, 陈苘, 黄百芬, 韩见龙
浙江省疾病预防控制中心,浙江 杭州 310051
Determination of bongkrekic acid in plasma of food poisoning patients by liquid chromatography-tandem mass spectrometry
XU Xiao-min, CHEN Qing, HUANG Bai-fen, HAN Jian-long
Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China
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摘要 目的 建立快速测定血浆中米酵菌酸的液相色谱-串联质谱法,为相关食源性中毒事件的病因学鉴定提供技术支持。方法 血浆样品经乙腈沉淀蛋白、水稀释、PAX阴离子交换固相萃取小柱净化后,采用XBridgeTM BEH C18色谱柱分离,0.01 %(v/v)氨水-甲醇为流动相梯度洗脱,采用液相色谱-串联质谱法检测血浆中米酵菌酸含量。结果 血浆中米酵菌酸在1~400 ng/mL浓度范围内线性关系良好,相关系数为0.999 3,线性回归方程为y=16 509x+3 134.3。方法 检出限为0.5 ng/mL,定量限为1 ng/mL。在1(定量限)、10(10倍定量限)、200 ng/mL(线性范围中间点)3个浓度水平下,加标平均回收率为76.0%~96.7%,相对标准偏差为5.2%~12.8%。检测2例食源性中毒患者血浆中米酵菌酸含量分别为394 ng/mL和92.3 ng/mL。结论 通过优化样品前处理和色谱分离条件,采用液相色谱-串联质谱法可以实现血浆中米酵菌酸快速准确的定性和定量分析,满足实际样品检测的需要。
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徐小民
陈苘
黄百芬
韩见龙
关键词 米酵菌酸液相色谱-串联质谱法PAX阴离子交换柱净化血浆    
AbstractObjective To quickly determine bongkrekic acid(BKA)in plasma qualitatively and quantitatively by liquid chromatography-tandem mass spectrometry(LC-MS/MS),and to provide technical support for etiological identification of food poisoning events. Methods The plasma sample was protein precipitated with acetonitrile,diluted with water and purified with anion exchange solid phase extraction cartridge of PAX. The sample extract was separated by an XBridgeTM BEH C18 chromatographic column. Gradient elution was conducted with the mobile phase of 0.01 %(v/v)ammonia and methanol. Then BKA was detected by LC-MS/MS. Results The equation of linear regression was y=16 509x+3 134.3. Good linear relationship was obtained for BKA at a range from 1 to 400 ng/mL in plasma,with the correlation coefficient of 0.999 3. The limit of detection(LOD)was 0.5 ng/mL and the limit of quantitation(LOQ)was 1 ng/mL. The average recoveries were 76.0%-96.7% with relative standard deviations(RSDs,n=6)of 5.2%-12.8% at three spiking levels of 1(LOQ),10(10 times of LOQ)and 200 ng/mL(medium of linear range). The concentrations of BKA in plasma obtained from two patients suffering from food poisoning were 394 and 92.3 ng/mL. Conclusion The optimized sample pretreatment and chromatographic separation conditions can achieve rapid,accurate,qualitative and quantitative analysis of BKA in plasma.
Key wordsBongkrekic acid    Liquid chromatography-tandem mass spectrometry    PAX anion exchange purification    Plasma
收稿日期: 2019-07-24      修回日期: 2019-08-16     
中图分类号:  R115  
基金资助:浙江省基础公益类科技计划(LGF18H260007); 浙江省食品安全检测技术中心(2015DZ002)
通信作者: 徐小民,E-mail:chemxuxm@163.com   
作者简介: 徐小民,博士,副主任技师,主要从事食品安全理化检验工作
引用本文:   
徐小民, 陈苘, 黄百芬, 韩见龙. 液相色谱-串联质谱法测定食源性中毒患者血浆中米酵菌酸[J]. 预防医学, 2019, 31(12): 1205-1209.
XU Xiao-min, CHEN Qing, HUANG Bai-fen, HAN Jian-long. Determination of bongkrekic acid in plasma of food poisoning patients by liquid chromatography-tandem mass spectrometry. Preventive Medicine, 2019, 31(12): 1205-1209.
链接本文:  
http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2019.12.004      或      http://www.zjyfyxzz.com/CN/Y2019/V31/I12/1205
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