作者：胡江涛1,2, 俞凌云1, 于刚1, 帅培强1, 张莹3, 吴孟茹1, 张琴1
作者单位：1. 四川出入境检验检疫局检验检疫技术中心, 四川 成都 610041;
2. 食品安全检测(四川省)重点实验室, 四川 成都 610041;
3. 宜宾出入境检验检疫局, 四川 宜宾 644000
关键词：柱前电化学衍生;孔雀石绿;隐性孔雀石绿;高效液相色谱
摘要：
建立柱前电化学氧化-高效液相色谱测定水产品中孔雀石绿(MG)及隐性孔雀石绿(LMG)残留量的方法。试样经乙酸铵缓冲液/乙腈提取,酸性氧化铝吸附剂净化,乙腈和乙酸铵缓冲液(78:22,:)等度洗脱,柱前600 mV电压下LMG被氧化衍生成MG,618 nm波长检测,测定结果为总量;当电压为0 mV时,结果仅为样品中MG含量。并在各自相应浓度范围内线性良好,相关系数不低于0.996,三水平加标平均回收率为76.0%～95.0%,相对标准偏差(RSD)为1.7%～8.6%。方法的检出限为2.0 g/kg,定量限为5.0 g/kg。方法精密度、准确度和检出限等性能指标均达到兽残分析的要求,可用于水产品中的孔雀石绿及隐性孔雀石绿的检测。
Etermination of malachite green and leucomalachite green residues in aquatic products by HPLC with per-column coulometric electrochemical derivation
HU Jiangtao1,2, YU Lingyun1, YU Gang1, SHUAI Peiqiang1, ZHANG Ying3, WU Mengru1, ZHANG Qin1
1. Sichuan Entry-exit Inspection and Quarantine Bureau Technical Center, Chengdu 610041, China;
2. Food Safety Testing Key Laboratory of Sichuan Province, Chengdu 610041, China;
3. Yibin Entry-exit Inspection and Quarantine Bureau, Yibin 644000, China
Abstract: A pre-column coulometric electrochemical derivation(PCED)-HPLC was developed to analyze the malachite Green and leucomalachite green left in aquatic products. Samples were extracted with ammonium acetate buffer and acetonitrile, purified with alumina-A adsorbent, and then eluted by gradient with a buffer prepared by 78 parts of acetonitrile and 22 parts of ammonium acetate. The leucomalachite green in the eluate was oxidized and derived into malachite green by a per-column coulometric electrochemical detector at 600 mV. Then, it was further detected at 618 nm to get the total amount of the two substances. When the voltage was 0 mV, the result presented the contents of malachite green in the sample. Calibration curves show a good linear relation in respective concentration range, with correlation coefficient no fewer than 0.996. The average recovery varies from 76.0% to 95.0% while the relative standard deviation (RSD) ranges from 1.7% to 8.6%. The limit of detection is 2.0 μg/kg, whereas the limit of quantitation is 5.0 μg/kg. The performance of the method such as precision, accurateness and detection limits can meet the requirements of testing of veterinary drug residues. Thus, it can be applied to detect the residues of malachite green and leucomalachite green in aquatic products.
Keywords: per-column coulometric electrochemical derivation;malachite green;leucomalachite green;high performance liquid chromatography
2016, 42(4): 49-53,64 收稿日期: 2015-12-13;收到修改稿日期: 2016-01-27
基金项目: 国家质检总局科技计划项目(2014IK137)
作者简介: 胡江涛(1974-),男,高级工程师,硕士,主要从事理化检验方面的研究。
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