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| Determination of Robenidine in Fishery Products by High Performance Liquid Chromatography with Dispersive Solid Phase Extraction |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:fishery products robenidine dispersive solid phase extraction high performance liquid chromatography（HPLC） |
| Author | Institution |
| 吴仕辉，陈昆慈，戴晓欣，马丽莎，朱新平，潘德博，郑光明，尹怡，谢文平 |
农业部水产种质监督检验测试中心（广州）中国水产科学研究院珠江水产研究所 |
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| Abstract: |
| A dispersive solid phase extraction coupled with high performance liquid chromatographic（HPLC） method was established for the determination of robenidine in fishery products.The sample was extracted with acidified ethyl acetate as extraction solvent and C18 as the sorbent，then purified by alumina-N.After evaporated to dryness，the residue was redissolved in acetonitrile water solution and defatted with n-hexane.The external standard method was used to quantify robenidine.The optimization chromatographic conditions were as follows：separation column：Agilent ODS-C18 chromatographic column（250 mm×4.6 mm，5 μm），mobile phase：pH 6.8 acetonitrile-ammonium dihydrogen phosphate buffer（65∶35，by volume），flow rate：1.0 mL/min，column temperature：40 ℃，sample volume：20 μL，detection wavelength：353 nm.Under the optimal conditions，the calibration curve showed a good linearity in the range of 0.01-1.00 mg/L with a correlation coefficient of 0.999 9.Four common representative samples（tilapia，eel，shrimp and turtle） were chosen for the validation of the method by recovery and precision.The obtained recoveries were 76%-106% and the relative standard deviations were 0.81%-8.2%.The limit of detection was 10 μg/kg，and the limit of quantitation was 30 μg/kg.Results of three inter-laboratory validation tests showed that the recoveries of robenidine in fish，shrimp and turtle samples at three spiked concentration levels were greater than 70% with relative standard deviations not more than 11%.With the advantages of simple operation，good sensitivity，accuracy and reproducibility，the proposed method was successfully used in the determination of robenidine in real samples,which can be recommended as the related test method for application. |
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