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| 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
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| Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China |
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Abstract Objective 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.
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Received: 24 July 2019
Revised: 16 August 2019
Published: 27 November 2019
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[1] MOEBIUS N,ROSS C,SCHERLACH K,et al.Biosynthesis of the respiratory toxin bongkrekic acid in the pathogenic bacterium burkholderia gladioli[J]. Chem Biol,2012,19(9):1164-1174.
[2] MATSUMOTO K,SUYAMA M,FUJITA S,et al.Efficient total synthesis of bongkrekic acid and apoptosis inhibitory activity of its analogues[J]. Chem Eur J,2015,21(32):11590-11602.
[3] 周鹏. 超高效液相色谱串联质谱法测定银耳中米酵菌酸[J]. 食品研究与开发,2015,36(22):123-126.
[4] FALCONER T M,KERN S E,BRZEZINSKI J L,et al.Identification of the potent toxin bongkrekic acid in a traditional African beverage linked to a fatal outbreak[J]. Forensic Sci Int,2017, 270:e5-e11.
[5] 周帼萍,梁泉,黄庭轩,等. 云南省文山州广南县吊浆粑食物中毒事件的病原学分析[J]. 中国食品卫生杂志,2017,29(1):71-75.
[6] 郭铃. 椰毒假单胞菌食物中毒实验室检测[J]. 现代预防医学,2007,34(6):1145-1147.
[7] 李红艳,金燕飞,黄海智,等. 高效液相色谱-二极管阵列检测器测定食品中米酵菌酸残留[J]. 食品科学,2016,37(24):247-251.
[8] 申慧慧,陈军辉,徐秀丽,等. 海产贝类脂溶性贝毒素的高效液相色谱-串联质谱分析方法及其食用安全性评价[J]. 分析化学,2018,46(6):985-992.
[9] 高何刚,杜赛,王瑞,等. 超高效液相色谱-串联质谱法测定蜂蜜中氯霉素和甲硝唑残留[J]. 预防医学,2017,29(9):969-972.
[10] 张晓艺,张秀尧,蔡欣欣,等. 超高效液相色谱联用三重四极杆质谱法同时测定蜂蜜中氯霉素、甲硝唑和林可霉素[J]. 预防医学,2019,31(2):212-216.
[11] 许娇娇,黄百芬,周健,等. 直接稀释-超高效液相色谱-串联质谱法快速测定谷物及其制品中16种真菌毒素[J]. 中国食品卫生杂志,2017,29(6):708-715.
[12] 王宗义,杨定忠,冀梦瑶,等. 高效液相色谱-串联质谱检测牛奶中的甲状腺素[J]. 色谱,2013,31(3):270-274.
[13] XU X M,CAI Z X,ZHANG J S,et al.Analysis of monofluoroacetic acid in urine by liquid chromatography-triple quadrupole mass spectrometry and preparation of the positive sample by the bioconversion from monofluoroacetamide to monofluoroacetic acid in vitro[J]. J Chromatogr B,2016,1027:131-138.
[14] 沈斐,许燕娟,姜晟,等. 超高效液相色谱-串联质谱法测定水华样品中微囊藻毒素及其基质效应的消除[J]. 色谱,2017, 35(7):772-777.
[15] 刘晓云,陈笑艳,钟大放. 液相色谱-串联质谱生物分析方法的基质效应和对策[J]. 质谱学报,2017,38(4):388-399.
[16] DESFONTAINE V,CAPETTI F,NICOLI R,et al.Systematic evaluation of matrix effects in supercritical fluid chromatography versus liquid chromatography coupled to mass spectrometry for biological samples[J]. J Chromatogr B,2018,1079:51-61.
[17] XU X M,YU X W,LU M,et al.Study of the matrix effects of tetrodotoxin and its content in cooked seafood by liquid chromatography with triple quadrupole mass spectrometry[J]. J Sep Sci,2015,38(19):3374-3382.
[18] 张程,严天,陈川,等. 氟固相萃取辅助的生物分子质谱分析新方法[J]. 分析化学,2017,45(12):1857-1864.
[19] 黄原飞,娄晓,周哲,等. 分子印迹聚合物固相萃取-超高效液相色谱-串联质谱法检测水产品中11种氨基糖苷类药物残留[J]. 分析化学,2018,46(3):454-461.
[20] 栾玉静,王瑞花,董颖,等. 固相萃取-液相色谱-质谱法检验人全血中的地塞米松[J]. 中国法医学杂志,2017,32(3):297-299. |
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