色谱

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毛细管气相色谱法测定南美白对虾中硫丹的残留量

刘晓松1,黄大新1,卢声宇2   

  1. 1.Guangxi Technology Center of Entry-Exit Inspection and Quarantine Bureau, Nanning 530021, China;
    2.Fujian Technology Center of Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350003, China
  • 收稿日期:2006-11-08 修回日期:2007-01-16 出版日期:2007-05-30 发布日期:1985-09-25
  • 通讯作者: 刘晓松

Determination of Endosulfan Pesticide Residues in Litopenaeus vannamai by Capillary Gas Chromatography

LIU Xiaosong1, HUANG Daxin1, LU Shengyu2   

  1. 1.Guangxi Technology Center of Entry-Exit Inspection and Quarantine Bureau, Nanning 530021, China;
    2.Fujian Technology Center of Entry-Exit Inspection and Quarantine Bureau, Fuzhou 350003, China
  • Received:2006-11-08 Revised:2007-01-16 Online:2007-05-30 Published:1985-09-25
  • Contact: LIU Xiaosong

摘要: 建立了运用毛细管气相色谱检测南美白对虾中硫丹残留的快速测定方法。用乙酸乙酯提取样品中的硫丹,提取液浓缩后以中性氧化铝和活性炭小柱进行双级柱色谱净化,用正己烷-乙酸乙酯(体积比为1∶1)洗脱,洗脱液用气相色谱-电子捕获检测器检测,以保留时间定性,外标法定量。在南美白对虾样品中分别添加0.20,0.10,0.04和0.02 mg/kg硫丹标准品,测得添加回收率为80.5%~109.5%,相对标准偏差为3.6%~8.4%。该方法在不具备凝胶渗透色谱条件下也能进行硫丹残留的检测,具有简便、准确的特点,能满足常规检测及食品安全监控的需要。

关键词: 残留量, 硫丹, 毛细管气相色谱法, 南美白对虾

Abstract: A method is described for the determination of endosulfan pesticide residues in Litopenaeus vannamai by capillary gas chromatography. The residues of α-endosulfan and β-endosulfan were extracted from the sample with ethyl acetate, and the extract was cleaned up using a neutral alumina column and an active carbon column after concentrated and then eluted with a mixture of n-hexane-ethyl acetate (1∶1, v/v). During the process of purification, the flow rate of eluent was controlled within 3 mL/min. The eluate was collected and evaporated to 1 mL for analysis. The determination was performed on a gas chromatograph equipped with an electron capture detector. The retention time was used for qualification and the external calibration standard was used for quantitation. The results obtained showed that the recoveries were 80.5%-97.3% for α-endosulfan and 81.1%-109.5% for β-endosulfan. The limit of detection (LOD) was 0.002 mg/kg, and the limit of quantitation (LOQ) was 0.007 mg/kg for both. The precision of the method, expressed as the relative standard deviation for the within-laboratory repeatability, was generally below 8.5%. The method was used for the analysis of Litopenaeus vannamai samples from Guangxi Province, a Litopenaeus vannamai aquiculture area in south China.

Key words: endosulfan, Litopenaeus vannamai , residue, capillary gas chromatography (CGC)