Rapid Qualitative and Quantitative Analysis of Bongkrekic Acid in Human Whole Blood by Ultra-High Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry
摘 要
采集疑似米酵菌酸中毒患者全血样品200 μL,加入已于-20 ℃冷冻的甲醇800 μL,振荡5 min,离心5 min,上清液按照优化的仪器工作条件分析。在Infinity Lab Poroshell 120 EC-C18色谱柱(150 mm×3.0 mm,2.7 μm)上以不同体积比的含10 mmol·L-1甲酸铵的0.1%(体积分数,下同)甲酸溶液和乙腈的混合溶液梯度洗脱分离米酵菌酸,以双喷射流电喷雾离子源负离子模式电离,以全离子采集一级质谱(MS1-Allions)模式定性鉴别,以基质匹配工作曲线法定量。结果显示,米酵菌酸的质量浓度在45~450 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为3.2 μg·L-1。对空白全血样品进行3个浓度水平的加标回收试验,回收率为82.6%~90.1%,测定值的相对标准偏差(n=6)为4.5%~5.6%。方法应用于疑似中毒患者全血样品的分析,检出了米酵菌酸(检出量为2 225 μg·L-1)。
Abstract
The whole blood sample from suspected bongkrekic acid poisoning patient was collected, and 800 μL of methanol precooled at -20 ℃ was added into 200 μL of sample. After shaking for 5 min, the mixture was centrifuged for 5 min, and the supernatant was analyzed by the optimal instrumental working conditions. The bongkrekic acid was separated on the Infinity Lab Poroshell 120 EC-C18 column (150 mm×3.0 mm, 2.7 μm) by gradient elution using mixed solutions composed of 0.1% (volumn fraction) formic acid solution containing 10 mmol·L-1 ammonium formate and acetonitrile at various volumn ratios, ionzed by double jet stream electric spray ion source with negative mode, identified by MS1-Allions mode, and quantitatively analyzed by matrix-matched working curve. It was shown that the linear relationship between values of mass concentration and peak area was kept in the range of 45-450 μg·L-1, with detection limit (3S/N) of 3.2 μg·L-1. Test for the spiked recovery was made on blank whole blood samples at three concentration levels, giving values of recovery in the range of 82.6%-90.1%, and RSDs (n=6) of the determined values ranged from 4.5% to 5.6%. The proposed method was applied to the analysis of the whole blood sample from a suspected poisoning patient, and the bongkrekic acid was detected with detection amount of 2 225 μg·L-1.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202302003
所属栏目 工作简报
基金项目 广州市卫生健康科技重大项目(2021A031003);广州市第十二人民医院高层次人才科研项目(KY2020YLX08)
收稿日期 2021/9/24
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备注周丽屏,高级工程师,博士,主要从事职业卫生检测及毒物鉴定工作
引用该论文: ZHOU Liping,GUO Jiaming,GUO Yaoping,CHEN Jiu,WANG Zhi. Rapid Qualitative and Quantitative Analysis of Bongkrekic Acid in Human Whole Blood by Ultra-High Performance Liquid Chromatography-Quadrupole Time-of-Flight Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(2): 142~147
周丽屏,郭嘉明,郭尧平,陈纠,王致. 超高效液相色谱-四极杆飞行时间质谱法快速定性、定量分析人全血中米酵菌酸[J]. 理化检验-化学分册, 2023, 59(2): 142~147
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参考文献
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【17】李红艳,金燕飞,黄海智,等.高效液相色谱-二极管阵列检测器结合固相萃取法快速测定食品中米酵菌酸残留[J].食品科学, 2016,37(24):247-251.
【18】苏永恒,张伟,张榕杰,等.固相萃取-高效液相色谱法测定食品中米酵菌酸含量[J].中国卫生工程学, 2017,16(4):438-439.
【19】李红娜,袁飞,张辰陽,等.液相色谱和飞行时间质谱联用检测米酵菌酸[J].食品工业, 2018,39,262(7):324-328.
【20】张秀尧,蔡欣欣,张晓艺,等.超高效液相色谱-三重四极杆质谱联用法测定血浆和尿液中米酵菌酸和异米酵菌酸[J].质谱学报, 2020,41(3):268-277.
【2】ANWAR M, KASPER A, STECK A R, et al. Bongkrekic acid-a review of a lesser-known mitochondrial toxin[J]. Journal of Medical Toxicology, 2017,13(2):1-7.
【3】HUANG Q, WU Z. Safe eating of fermented corn and coconut food:Mechanism, clinical manifestations and inhibition of food poisoning involved in bongkrekic acid[J]. E3S Web of Conferences, 2021,267(10):2075.
【4】GUDO E S, COOK K, KASPER A M, et al. Description of a mass poisoning in a rural district in mozambique:The first documented bongkrekic acid poisoning in africa[J]. Clinical Infectious Diseases, 2018,66(9):1400-1406.
【5】杨果平.谨防米酵菌酸中毒,避免"酸汤子"悲剧重演[J].食品与健康, 2021,4:56-57.
【6】刘秀梅.我国椰毒假单胞菌酵米面亚种食物中毒流行趋势浅析[J].中华预防医学杂志, 1996,30(6):372-374.
【7】梁玉裕,唐振柱,沈莹,等.广西1996-2005年酵米面食物中毒情况分析[J].中国食品卫生杂志, 2006,18(6):544-545.
【8】吴险峰,曲刚.酵米面食物中毒致死3例报道[J].内蒙古中医药, 1999(1):20-20.
【9】苏继凤,王灿永.霉米面中毒39例报告[J].中国临床医生杂志, 2003,31(6):30-31.
【10】刘志涛,万蓉,胡太芬,等.一起椰毒假单胞菌酵米面亚种引起的食物中毒调查分析[J].职业与健康, 2013,29(5):582-583.
【11】申屠平平,朱珈慧,徐小民,等.一起椰毒假单胞菌酵米面亚种引起的食物中毒调查[J].上海预防医学, 2019,31(6):466-468.
【12】王德清,于天林,陈永禄.食变质银耳中毒——附22例报告[J].河南诊断与治疗杂志, 1997,(1):51-52.
【13】张俊梅.一起因食用变质银耳引起的椰毒假单孢菌酵米面亚种食物中毒调查报告[J].中国医药指南, 2015,3:286-287.
【14】王连伟,高立功.变质银耳中毒5例[J].中西医结合实用临床急救, 1996,3(7):F003.
【15】王海燕,宋曼丹,王建,等.广东省首起米粉米酵菌酸中毒病原菌鉴定研究[J].中国食品卫生杂志, 2019,31(4):394-398.
【16】任琳,秦忠雪,胡彬,等.尿样中米酵菌酸高效液相色谱法测定[J].中国公共卫生, 2020,36(3):439-440.
【17】李红艳,金燕飞,黄海智,等.高效液相色谱-二极管阵列检测器结合固相萃取法快速测定食品中米酵菌酸残留[J].食品科学, 2016,37(24):247-251.
【18】苏永恒,张伟,张榕杰,等.固相萃取-高效液相色谱法测定食品中米酵菌酸含量[J].中国卫生工程学, 2017,16(4):438-439.
【19】李红娜,袁飞,张辰陽,等.液相色谱和飞行时间质谱联用检测米酵菌酸[J].食品工业, 2018,39,262(7):324-328.
【20】张秀尧,蔡欣欣,张晓艺,等.超高效液相色谱-三重四极杆质谱联用法测定血浆和尿液中米酵菌酸和异米酵菌酸[J].质谱学报, 2020,41(3):268-277.
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