张月, 吕岱竹, 韩丙军, 林靖凌. 超高效液相色谱-串联质谱法测定咖啡鲜果中草铵膦及其代谢产物残留[J]. 农药学学报, 2014, 16(6): 734-739. DOI: 10.3969/j.issn.1008-7303.2014.06.16
    引用本文: 张月, 吕岱竹, 韩丙军, 林靖凌. 超高效液相色谱-串联质谱法测定咖啡鲜果中草铵膦及其代谢产物残留[J]. 农药学学报, 2014, 16(6): 734-739. DOI: 10.3969/j.issn.1008-7303.2014.06.16
    ZHANG Yue, LÜ Daizhu, HAN Bingjun, LIN Jingling. Determining residues of glufosinate-ammonium and its metabolites in coffee cherries by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2014, 16(6): 734-739. DOI: 10.3969/j.issn.1008-7303.2014.06.16
    Citation: ZHANG Yue, LÜ Daizhu, HAN Bingjun, LIN Jingling. Determining residues of glufosinate-ammonium and its metabolites in coffee cherries by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Pesticide Science, 2014, 16(6): 734-739. DOI: 10.3969/j.issn.1008-7303.2014.06.16

    超高效液相色谱-串联质谱法测定咖啡鲜果中草铵膦及其代谢产物残留

    Determining residues of glufosinate-ammonium and its metabolites in coffee cherries by ultra performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了咖啡鲜果中草铵膦(glufosinate-ammonium)及其代谢产物N-乙酰草铵磷(N-acetyl-glufosinate)和 3-(甲基膦基)丙酸(3-hydroxy(methyl) phosphinoyl)的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。样品经0.1 mol/L的氨水匀浆、超声提取、离心后,取上清液于40 ℃下减压浓缩,以V(甲醇):V (水)=1:1的混合溶剂定容,经ACQUITY UPLC BEH HILIC色谱柱分离,以乙腈-0.1%甲酸水溶液混合溶剂为流动相梯度洗脱,采用多离子反应监测(MRM)模式扫描,外标法定量。结果表明:在0.1~2.0 mg/L质量浓度范围内,3种化合物的进样浓度与其峰面积之间呈良好线性相关,相关系数(r)分别为0.997、0.998和0.991;在0.05~0.5 mg/kg水平下进行添加回收试验,3种化合物的回收率在92% ~107%之间,相对标准偏差(RSD)在 2.0% ~4.9%之间,定量限(LOQ)均为0.05 mg/kg。该方法简化了样品前处理,提高了回收率,适用于草铵膦的残留检测。

       

      Abstract: A ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the determination of glufosinate-ammonium and its metabolites in coffee cherries was established. The samples were thoroughly homogenized and ultrasonic extracted with 0.1 mol/L ammonia water. After centrifugation, the supernatant was concentrated at 40 ℃, and dissolved with methanol-water solution (V:V=1:1). The sample solutions were separated by an ACQUITY UPLC BEH HILIC column with gradient elution in aqueous solution containing 0.1% formic acid, and detected on a tandem mass spectrometry operated in multi-reaction monitoring (MRM) mode and quantified with external standards. The results showed that the calibration curve was linear within the range of 0.1-2.0 mg/L with correlation coefficient(r) of 0.997, 0.998 and 0.991, respectively. The average recoveries of 3 compounds were 92%-107% at spiked levels from 0.05 mg/kg to 0.5 mg/kg, with relative standard deviations (RSD) between 2.0% and 4.9%. The limit of quantification(LOQ) was 0.05 mg/kg. The method simplifies the pretreatment, improves the recovery, and is suitable for the analysis of glufosinate-ammonium residue.

       

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