色谱

色谱

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高效液相色谱-串联质谱法测定多种农产品中杀草强的残留量

李立1*, 付建2, 高洪良2, 任海涛3, 娄喜山2, 管立辉3   

  1. 1. 中国检验检疫科学研究院, 北京 100123; 2. 烟台杰科检测服务有限公司, 山东 莱阳 265231; 3. 莱阳恒润食品有限公司, 山东 莱阳 265200
  • 收稿日期:2009-08-18 修回日期:2009-10-18 出版日期:2010-03-28 发布日期:1981-03-25
  • 通讯作者: 李立

Determination of amitrole in agricultural products by high performance liquid chromatography-tandem mass spectrometry

LI Li1*, FU Jian2, GAO Hongliang2, REN Haitao3, LOU Xishan2, GUAN Lihui3   

  1. 1. Chinese Academy of Inspection and Quarantine, Beijing 100123, China; 2. Yantai Jieke Inspection Co. Ltd, Laiyang 265231, China; 3. Laiyang Hengrun Foodstaff Co. Ltd, Laiyang 265200, China
  • Received:2009-08-18 Revised:2009-10-18 Online:2010-03-28 Published:1981-03-25
  • Contact: LI Li

PDF

683

被引次数

9

摘要： 建立了采用高效液相色谱-串联质谱法(HPLC-MS/MS)检测多种农产品中杀草强残留量的方法。根据样品基质不同,分别采用25%丙酮水溶液(针对小麦、鱼、肉和肝脏样品)、1%乙酸酸化的25%丙酮水溶液(针对玉米和花生样品)、1%乙酸水溶液(针对金银花、姜粉、花椒粉和茶叶样品)及1%乙酸水溶液和二氯甲烷(针对苹果、菠萝、菠菜、胡萝卜和紫苏叶）进行提取,然后依次采用二氯甲烷萃取、PCX或ENVI-Carb固相萃取柱净化后,进行HPLC-MS/MS测定,外标法定量。在0.005～0.1 mg/kg范围内,杀草强的峰面积与其质量浓度有良好的线性关系,相关系数为0.9997。对上述15种不同种类的农产品进行添加回收,回收率为67.5%~98.1%,相对标准偏差为1.0%~9.8%。苹果、菠菜、紫苏叶、玉米、姜、鱼和肉等样品的定量限为0.01 mg/kg,茶叶、金银花、花椒粉的定量限为0.02 mg/kg。该方法的灵敏度、准确度和精密度均符合农药残留测定的技术要求。

关键词: 高效液相色谱-串联质谱法, 固相萃取, 农产品 , 杀草强

Abstract: A high performance liquid chromatography-tandem mass spectrometry method (HPLC-MS/MS) was developed for the analysis of amitrole residues in agricultural products. The samples were extracted by 25% acetone for wheat, fish, pork and liver samples, 1% acetic acid-25% acetone for maize and peanut samples, 1% acetic acid solution for honeysuckle, the powder of ginger, the powder of bunge prickly ash and tea leaves samples, 1% acetic acid solution-dichloromethane for apple, pineapple, spinach, carrot, perilla leaves samples, respectively, followed by liquid-liquid extraction with dichloromethane. The samples were then cleaned up by PCX or Envi-Carb solid-phase extraction cartridge. The amitrole was determined and confirmed by HPLC-MS/MS. The results showed a linear relationship in the range of 0.005－0.1 mg/kg for amitrole. The correlation coefficient was 0.9997. The average recoveries of amitrole in wheat, maize, peanut, pineapple, apple, carrot, spinach, pork, the powder of ginger, the powder of bunge prickly ash, perilla, liver, fish, honeysuckle and tea were 67.5%－98.1%. The relative standard deviations (RSDs) were 1.0%－9.8%. The limits of quantitation were 10μg/kg for wheat, maize, peanut, pineapple, apple, carrot, spinach, pork, perilla, liver, fish, honeysuckle and 20μg/kg for the powder of bunge prickly ash, the powder of ginger and tea, respectively. The method is simple, sensitive and accurate.

Key words: agricultural products , amitrole, solid-phase extraction (SPE), high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)