Determination of Residues of Ochratoxin A and B in Wine by LC-MS/MS
摘 要
采用液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A、B的残留量。样品用氨水调节pH后离心,上清液过C18固相萃取柱净化,以甲醇洗脱,氮气吹至近干后用甲醇-0.15%甲酸(7+3)溶液定容至1 mL。以Agilent Eclipse XDB-C18色谱柱为分离柱,以甲醇-含5 mmol·L-1乙酸铵溶液的0.15%甲酸溶液(7+3)混合液为流动相进行洗脱,采用电喷雾离子源及选择多反应监测模式进行测定。赭曲霉毒素A、B的线性范围在10.0 μg·L-1以内,方法的测定下限(10S/N)均为2.0 μg·L-1。对空白样品进行加标回收试验,回收率在66.3%~87.4%之间,测定值的相对标准偏差(n=6)在5.2%~7.6%之间。方法用于葡萄酒中赭曲霉毒素A、B的测定, 结果与美国化学家协会检测方法的测定结果一致。
Abstract
A method of LC-MS/MS was applied to determine residues of ochratoxin A and B in wine. The sample was centrifuged after pH was adjusted. The supernatant was purified using C18 SPE column with methanol as eluent. The eluate was evaporated to dryness by N2 blowing, and the residue was dissolved in 1 mL of mixture of methanol-0.15% (φ) formic acid (7+3) solution. Agilent Eclipse XDB-C18 column was used as stationary phase and the mixture of methanol-0.15% (φ) formic acid (7+3) solution (with 5 mmol·L-1 NH4Ac) was used as mobile phase for elution. ESI and MRM were adopted in MS/MS detection. The linearity ranges of ochratoxin A and B were found below 10.0 μg·L-1, with lower limits of determination (10S/N) of 2.0 μg·L-1. Recovery measured by standard addition method was in the range of 66.3%-87.4% with RSD′s (n=6) in the range of 5.2%-7.6%. The method was applied for the determination of residual of ochratoxin A and B in wine, giving results consistent with that obtained by the AOAC method.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201509020
所属栏目 工作简报
基金项目 浙江省重点科技创新团队(2010R50028);质检总局 科技计划(2013IK188)
收稿日期 2014/8/12
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备注侯建波(1983-),男,满族,内蒙古人,高级工程师, 博士,研究方向食品中药物残留分析。
引用该论文: HOU Jian-bo,XIE Wen,LI Jie,LV Chun-hua,SHEN Wei-feng,HE Jian-min. Determination of Residues of Ochratoxin A and B in Wine by LC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(9): 1290~1293
侯建波,谢文,李杰,吕春华,沈炜锋,何建敏. 液相色谱-串联质谱法测定葡萄酒中赭曲霉毒素A、B的残留量[J]. 理化检验-化学分册, 2015, 51(9): 1290~1293
被引情况:
【1】邱丰艳,丁力,陈雪梅, "超高效液相色谱-串联四极杆质谱法测定鸡腿菇中4-己基间苯二酚的含量",理化检验-化学分册 52, 514-517(2016)
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参考文献
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【7】熊勇华,陈雪岚,许杨.检测赭曲霉毒素A(OTA)的酶联免疫吸附法(ELISA)体系的建立[J].食品科学, 2006,27(5):30-35.
【8】康健,钟其顶,熊正河,等.葡萄酒中赭曲霉素A测定方法的研究[J].食品与发酵工业, 2009,35(3):153-157.
【9】REINSCH M, TPFER A, LEHMANN A, et al. Determination of ochratoxin a in beer by LC-MS/MS ion trap detection[J]. Food Chemistry, 2007,100(1):312-317.
【10】阎龙宝,王浩.液相色谱-质谱联用技术测定葡萄酒中的赭曲霉毒素A残留[J].食品研究与开发, 2010,31(6):136-138.
【2】GB/T 5009 96-2003 谷物和大豆中赭曲霉毒素A的测定[S].
【3】VISCONTI A, PASCALE M, CENTONZE G. Determination of ochratoxin a in wine and beer by immunoaffinity column cleannup and liquid chromatographic analysis with fluorometric detection: collaborative study[J]. Journal of AOAC International, 2001,84(6):1818-1827.
【4】宗腩,李景明,张柏林.检测葡萄酒中赭曲霉毒素A的SPE-HPLC方法优化[J].中国酿造, 2011,4:32-35.
【5】马晓旭,马丽艳,杨丽丽,等.C18固相萃取柱-高效液相色谱法测定葡萄干中赭曲霉毒素A, 2012,31(7):64-67.
【6】BEATRIZ P S, MONICA C, JEAN-LOUIS M, et al. Novel highly-performing immunosensor-based strategy for ochratoxin a detection in wine samples[J]. Biosensors and Bioelectronics, 2008,23:995-1002.
【7】熊勇华,陈雪岚,许杨.检测赭曲霉毒素A(OTA)的酶联免疫吸附法(ELISA)体系的建立[J].食品科学, 2006,27(5):30-35.
【8】康健,钟其顶,熊正河,等.葡萄酒中赭曲霉素A测定方法的研究[J].食品与发酵工业, 2009,35(3):153-157.
【9】REINSCH M, TPFER A, LEHMANN A, et al. Determination of ochratoxin a in beer by LC-MS/MS ion trap detection[J]. Food Chemistry, 2007,100(1):312-317.
【10】阎龙宝,王浩.液相色谱-质谱联用技术测定葡萄酒中的赭曲霉毒素A残留[J].食品研究与开发, 2010,31(6):136-138.
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