LC-MS/MS Determination of 4 Food Borne Plant Toxins in Blood
摘 要
采用液相色谱-串联质谱法测定血中毒芹碱、金雀花碱、秋水仙碱和α-茄碱等4种食源性植物毒素的含量。0.2 mL血样用0.8 mL乙腈去除血红蛋白,离心后,上层清液经0.22 μm有机系微孔滤膜过滤。以Hypurity C18色谱柱为分离柱,0.2%(体积分数)乙酸溶液(含有5 mmol·L-1乙酸铵,pH为4.0)和甲醇(20+80)的混合液为流动相进行等度洗脱,串联质谱分析中采用全扫描和选择反应监测模式。4种食源性植物毒素的质量浓度均在5.0~500 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)均为2.0 μg·L-1,测定下限(10S/N)均为5.0 μg·L-1。在50,200,500 μg·L-1等3个浓度水平进行加标回收试验,回收率为84.5%~111%,测定值的相对标准偏差(n=5)为1.5%~6.2%。
Abstract
LC-MS/MS was applied to the determination of 4 food borne plant toxins, i.e. coniine, cytisine, colchicine and solanine alkaloids in blood. Hemoglobin in 0.2 mL of blood sample was removed with 0.8 mL of acetonitrile. After centrifugation,the supernatant was filtered on 0.22 μm organic microporous filter membrane. Hypurity C18 chromatographic column was used as stationary phase, and the mixture of 0.2% (φ) acetic acid solution (containing 5 mmol·L-1 ammonium acetate, pH was 4.0) and methanol (20+80) was used as mobile phase in isometric elution. The full scanning mode and the selected reaction monitoring mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 4 food borne plant toxins were kept in the same range of 5.0-500 μg·L-1, with the same detection limit (3S/N) of 2.0 μg·L-1 and the same lower limit of determination (10S/N) of 5.0 μg·L-1. Tests for recovery were made by standard addition method at the concentration levels of 50, 200, 500 μg·L-1, giving values of recovery and RSDs (n=5) in the ranges of 84.5%-111% and 1.5%-6.2% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201811013
所属栏目 工作简报
基金项目 2016年国家级大学生创新训练计划项目(201610175049)
收稿日期 2017/12/1
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备注张婷,副教授,博士,研究方向为刑事毒物、毒品分析,zhangting_sy@sina.cn
引用该论文: ZHANG Ting,LIU Yafeng,SUN Ce,ZHAO Xintong. LC-MS/MS Determination of 4 Food Borne Plant Toxins in Blood[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(11): 1299~1302
张婷,刘亚峰,孙册,赵欣彤. 液相色谱-串联质谱法测定血中4种食源性植物毒素[J]. 理化检验-化学分册, 2018, 54(11): 1299~1302
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参考文献
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【3】汪乃兴,赵滨,邵丙锐.秋水仙碱传感器的研制及分析应用[J].化学传感器, 1993,13(1):71-74.
【4】ZHANG H. Electrochemistry and voltammetric determination of colchicine using an acetylene black-dihexadecyl hydrogen phosphate composite film modified glassy carbon electrode[J]. Bioelectrochemistry, 2006,68(2):197-201.
【5】黄少平.高效毛细管电泳法在药物分析及体内分析中的应用[J].中华临床医学研究杂志, 2016,12(9):1246-1249.
【6】李文杰,张林军,张冬梅,等.金雀花碱的波谱特征与结构确证[J].化学分析计量, 2013,22(3):36-40.
【7】陈旻,陈英.HPLC测定秋水仙碱片的含量及含量均匀度[J].中国现代应用药学, 2010,27(2):141-143.
【8】邵慧凯,丘汾,何佳平,等.异丁醇萃取-高效液相色谱法测定马铃薯中α-茄碱[J].中国食品卫生杂志, 2015,27(5):517-520.
【9】周军辉,石新卫,崔新爱,等.HPLC法测定披针叶黄华不同部位中金雀花碱及其衍生物的含量[J].药物分析杂志, 2014,34(10):1737-1740.
【10】BEYER J, PETERS F T, KRAEMER T, et al. Detection and validated quantification of toxic alkaloids in human blood plasma-comparison of LC-APCI-MS with LC-ESI-MS/MS[J]. Journal of Mass Spectrometry, 2007,42(5):621-633.
【11】伍慧敏,曾静,李美,等.液相色谱-质谱联用法检测马铃薯中α-茄碱含量[J].食品科学, 2013,34(24):121-124.
【12】张秀尧,蔡欣欣,张晓艺.超高效液相色谱-三重四极杆质谱联用方法测定血浆和尿液中的α-龙葵碱、α-卡茄碱和茄啶[J].色谱, 2014,32(6):586-590.
【13】赵建波,张丽慧,邱相君,等.高效液相色谱质谱检测血浆秋水仙碱及其药动学研究[J].杭州师范学院学报(医学版), 2007,27(6):349-352.
【14】DEVEAUX M, HUBERT N, DEMARLY C. Colchicine poisoning:Case report of two suicides[J]. Forensic Science International, 2004,143(2/3):219-222.
【15】陈晓红,仇佩虹,金米聪.高效液相色谱-质谱联用法同时测定体液中麻黄碱和秋水仙碱[J].理化检验-化学分册, 2006,42(10):790-793.
【16】刘伟,沈敏,沈保华,等.液相色谱-串联质谱法测定血液和尿液中秋水仙碱[J].中国法医学杂志, 2009,24(1):4-7.
【17】马晓斐,梁天佐,宋炜,等.高效液相色谱-串联质谱法同时测定中草药饮料中11种有毒生物碱[J].食品科学, 2014,35(8):226-230.
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