| 超高效液相色谱-串联质谱法测定甘蓝中三乙膦酸铝的残留 |
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投稿时间：2016-12-05
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| 引用本文：韩丙军,何燕,林冰,等.超高效液相色谱-串联质谱法测定甘蓝中三乙膦酸铝的残留[J].农药学学报,2017,19(3):403-408. |
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| 基金项目:海南省应用技术研发与示范推广专项（ZDXM2015044）；海南自然科学基金面上项目（20163078）；海南省高等学校科学研究项目（Hnky2016ZD-14）；中国热带农业科学院基本科研业务费专项资金（1630082017005） |
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| 中文摘要:建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）检测甘蓝中三乙膦酸铝残留的方法。通过测定甘蓝样品中乙基磷酸和亚磷酸的含量，对三乙膦酸铝进行定量。采用电喷雾负离子（ESI-）电离，多反应监测模式（MRM）定性分析，基质匹配标准曲线外标法定量。结果表明：三乙膦酸铝在不同配比的乙腈-水溶液中均可解离为乙基磷酸和亚磷酸，且二者的质量比均为40：60；三乙膦酸铝的检出限（LOD）为1.3 μg/kg；在10~500 μg/L范围内，乙基磷酸和亚磷酸的线性相关系数均大于0.999；在0.01、0.1和0.5 mg/kg 3个添加水平下，甘蓝中三乙膦酸铝的平均回收率在82%~107%之间，相对标准偏差（RSD）在6.7%~9.2%（n=5）之间。该方法简单、快速，灵敏度及准确度高，可满足甘蓝中三乙膦酸铝残留的检测要求。 |
| 中文关键词:超高效液相色谱-串联质谱 甘蓝 三乙膦酸铝 残留 乙基磷酸 亚磷酸 |
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| Determination of fosetyl-aluminium residue in cabbage (Brassica oleraceae L.) by using ultra-high performance liquid chromatography-tandem mass spectrometry |
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| Abstract:A rapid method for analyzing the fosetyl-aluminium (Al) residues in Chinese cabbage was developed using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). This method quantified the concentration of fosetyl-Al by determining the contents of ethyl phosphonic acid and phosphorous acid. Analytes were detected by electro-spray ionization (ESI-) and multiple reaction monitoring (MRM) mode. Fosetyl-Al dissociated as ethyl phosphonic acid and phosphoous acid, and the ratios between the two acids were 40:60 with different solution. Quantification was performed by peak area external standard methods using matrix-matched calibration curves, which were linear in the range of 10-500 μg/L with good linear relationships. The correlation coefficients were better than 0.999. The limit of quantification (LOQ) of fosetyl-Al was 1.3 μg/kg. At 0.01, 0.10 and 0.50 mg/kg spiked levels, the recoveries and the relative standard deviations (RSD) were 82%-107% and 6.7%-9.2% (n=5) for fosetyl-Al. This method was simple, rapid, accurate, which could be applied to the determination of fosetyl-Al residues in Chinese cabbage. |
| Key words:ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) cabbage fosetyl-aluminium residue ethyl phosphonic acid phosphorous acid |
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