玉米及其制品和小麦及其制品中白僵菌素和恩镰孢菌素的高效液相色谱-串联质谱检测方法的建立
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(国家食品安全风险评估中心 卫生部食品安全风险评估重点实验室,北京 100021)

作者简介:

韩小敏 女 副研究员 研究方向为食品卫生 E-mail:hanxiaomin@cfsa.net.cn通信作者:李凤琴 女 研究员 研究方向为食品卫生 E-mail:lifengqin@cfsa.net.cn

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基金项目:

科技基础工作专项(2013FY113400);北京市自然科学基金(7163235)


Development of high performance liquid chromatography tandem-mass spectrometry method for determination of beauvericin and enniatins in corn and wheat and their products
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(Key Laboratory of Food Safety Risk Assessment of Ministry of Health,China National Center for Food Safety Risk Assessment,Beijing 100021,China)

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    摘要:

    目的 建立了玉米及其制品和小麦及其制品中白僵菌素(beauvericin,BEA)、恩镰孢菌素A(enniatin A,ENA)、恩镰孢菌素A1(enniatin A1,ENA1)、恩镰孢菌素B(enniatin B,ENB)和恩镰孢菌素B1(enniatin B1,ENB1)的高效液相色谱-串联质谱检测方法。方法 样品经乙腈-水(85∶15,V/V)提取、室温静置、固相萃取柱净化后,以2 mmol/L乙酸铵水-乙腈作为流动相,采用电喷雾电离正离子多反应监测模式进行检测。结果 该方法对玉米及其制品和小麦及其制品中BEA和4种恩镰孢菌素(ENNs)的检出限范围分别为0.01~0.12和0.02~0.21 μg/kg,定量限范围分别为0.02~0.44和0.05~0.68 μg/kg,平均加标回收率范围分别为91.6%~149.7%和100.5%~128.2%,基质抑制或增强效应分别为88.0%~101.5%和55.8%~106.5%,且BEA和4种ENNs在所测基质中线性关系和精密度良好,相关系数均>0.99,相对标准偏差均<15%。结论 所建立的方法操作简便、灵敏度高、准确性好,可用于玉米及其制品和小麦及其制品中BEA和4种ENNs的测定。

    Abstract:

    Objective A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) for determination of beauvercin (BEA), enniatin A (ENA), enniatin A1 (ENA1), enniatin B (ENB) and enniatin B1 (ENB1) in corn, wheat and their products was developed. Methods Samples were extracted with acetonitrile-water (85∶15, V/V), cleaned up with solid phase extraction column followed by HPLC-MS/MS determination with electrospray positive ionization (ESI+) under multiple reaction monitoring (MRM) mode, and with 2 mmol/L ammonium acetate water-acetonitrile as the mobile phase. Results The limits of detection for BEA and 4 kinds of enniatins (ENNs) ranged from 0.01 to 0.12 μg/kg for corn and corn products and 0.02 to 0.21 μg/kg for wheat and wheat products, and the limits of quantification ranged from 0.02 to 0.44 μg/kg and 0.05 to 0.68 μg/kg for both cereals. The mean recoveries ranged from 91.6% to 149.7% for corn and corn products and 100.5% to 128.2% for wheat and wheat products, respectively. The matrix induced suppression or enhancement effect ranged from 88.0% to 101.5% and 55.8% to 106.5% for both cereals, respectively. The method for BEA and ENNs determination showed good linearity and precision in all matrixes with correlation coefficient above 0.99, and the relative standard deviations were less than 15%. Conclusion The method developed was of simple operation, high sensitivity and good accuracy, which could be used for BEA and 4 kinds of ENNs determination in corn and wheat and their products.

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韩小敏,徐文静,赵熙,张宏元,张靖,李凤琴.玉米及其制品和小麦及其制品中白僵菌素和恩镰孢菌素的高效液相色谱-串联质谱检测方法的建立[J].中国食品卫生杂志,2017,29(6):633-640.

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  • 收稿日期:2017-11-24
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  • 在线发布日期: 2018-01-29
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