固相萃取-高效液相色谱-荧光检测法测定水产品中4种丁香酚类化合物
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(1.国家海产品质量监督检验中心(湛江),广东 湛江 524094;2.广东海洋大学食品科技学院, 广东 湛江 524088;3.广东省湛江市质量计量监督检测所,广东 湛江 524094)

作者简介:

高平 男 高级工程师 研究方向为食品检测技术 E-mail:gaoyang2008694@126.com通信作者:┣┣(中)通信作者┫┫黄和 男 教授 研究方向为食品质量与安全 E-mail:zjhahe@163.com

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基金项目:

国家质检总局科技计划项目(2013QK272);广东省科技计划项目(2014A020208121)


Determination of four eugenol derivatives in aquatic products by SPE-HPLC-FLD
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(National Marine Products Quality Supervision and Inspection Center (Zhanjiang),Guangdong Zhanjiang 524094,China)

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    摘要:

    建立固相萃取-高效液相色谱荧光法测定水产品中4种丁香酚类化合物(丁香酚、异丁香酚、甲基丁香酚、甲基异丁香酚)残留的方法。方法 样品用乙腈提取,中性氧化铝和C18固相萃取柱净化,Inertsil ODS-SP C18柱(4.6 mm×250 mm,5 μm)分离,以甲醇-乙腈(1∶1,V/V)和1%冰乙酸水溶液为流动相,荧光检测激发波长为280 nm,发射波长为320 nm,外标法定量。结果 4种丁香酚类化合物在各自范围内线性关系良好,相关系数均>0.999,方法检出限为3.0~6.0 μg/kg,方法定量限为10.0~20.0 μg/kg,平均加标回收率为74.7%~103.0%,相对标准偏差(RSD)为2.6%~8.1%。结论 本方法操作简便、灵敏度高、实用性强,适用于水产品中丁香酚、异丁香酚、甲基丁香酚、甲基异丁香酚的残留分析检测。

    Abstract:

    A method was developed for the simultaneous determination of four eugenol derivatives residues(eugenol, isoeugenol, methyl eugenol, methyl isoeugenol) in aquatic products by solid-phase extraction-high performance liquid chromatography with fluorescence detection.Methods The samples were extracted by acetonitrile. The extracted solutions were cleaned up by neutral alumina coupled with C18 solid-phase extraction column. The target compounds were separated on a reversed phase C18 column using methanol-acetonitrile and 1% acetic acid as mobile phase, detected by the fluorescence detector at an excitation wavelength of 280 nm and an emission wavelength of 320 nm. External standard method was applied for quantitative analysis. Results The calibration curves of four eugenol derivatives showed good linearity within their respective linear ranges and high correlation coefficients (r>0.999). The limits of detection and the limits of qualification were 3.0-6.0 and 10.0-20.0 μg/kg, respectively.The average recoveries were in the range of 74.7%-103.0% with the relative standard deviations (RSDs) of 2.6%-8.1%. Conclusion The method was simple, highly sensitive and practical. It was suitable for the determination of eugenol, isoeugenol, methyl eugenol and methyl isoeugenol residues in aquatic products.

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高平,黄和,刘文侠,黄国方,李志清,杨嘉丽,陈焕.固相萃取-高效液相色谱-荧光检测法测定水产品中4种丁香酚类化合物[J].中国食品卫生杂志,2016,28(1):56-61.

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  • 收稿日期:2015-10-13
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  • 在线发布日期: 2016-02-19
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