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首页> 外文期刊>Journal of Agricultural and Food Chemistry >Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometric Determination of Quassin and Neoquassin in Fruits and Vegetables
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Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometric Determination of Quassin and Neoquassin in Fruits and Vegetables

机译：液相色谱电喷雾串联质谱法测定水果和蔬菜中的槲皮素和新quasassin

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摘要

Quassia amara wood chips are used by organic farmers as a valid alternative to synthetic insecticides. The powder of Q. amara contains high levels of quassin, neoquassin and picrasino-side B. In this study we developed a liquid chromatography mass spectrometry method for the rapid and accurate quantification of the insecticide quassinoids on fruits and vegetables. Quassinoids were extracted from fruits and vegetables with acetonitrile and separated on a Zorbax Column Eclipse XDB C8 by isocratic elution with a mobile phase consisting of water and methanol with 0.1% of formic acid. Using a high-performance liquid chromatograph coupled with an electrospray ionization tandem mass spectrometer (HPLC/ESI-MS/MS), quassinoids were selectively and simultaneously detected monitoring the multiple reaction (MRM) transitions of proton adduct precursor ions: m/z 389.5 → 222.9 for quassin, 391.5 → 372.9 for neoquassin and 576.1 → 394.5 for picrasinoside B. For all quassinoids calibration was linear over a working range of 1 and 100 μg/kg with r > 0.991. Limit of determination (LOD) and limit of quantification (LOQ) for both quassinoids were 0.5 and 1 μg/kg respectively while for picrasinoside B they were 5 and 10 μg/kg. Quassinoid recoveries ranged from 85.3% to 105.3% with coefficients of variation between 2.5% and 12.8% for fruit and vegetables. The presence of interfering compounds in the fruit and vegetable extract was evaluated and found to be minimal. Due to the linear behavior it was concludedthat the multiple reaction transitions of precursor ions can be used for analytical purposes, i.e. for identification and quantification of quassin, neoquassin, and picrasinoside B in fruit and vegetable extracts at trace levels.
机译：Quassia amara木片被有机农用作合成杀虫剂的有效替代品。 Q. amara的粉末中含有大量的quassin，新quassin和picrasino侧B。在这项研究中，我们开发了一种液相色谱质谱法，用于对水果和蔬菜上的农药类quasinoids进行快速，准确的定量。用水果中的乙腈从水果和蔬菜中提取类南瓜素，并在Zorbax Eclipse XDB C8色谱柱上进行等度洗脱，其流动相由水和甲醇以及0.1％的甲酸组成。使用高效液相色谱仪结合电喷雾电离串联质谱仪（HPLC / ESI-MS / MS），选择性地同时检测类胡萝卜素，从而监测质子加合物前体离子的多个反应（MRM）跃迁：m / z 389.5→ quassin的222.9，picosinoside B的新quassin的391.5→372.9和picrasinoside B的576.1→394.5。对于所有的类quasinoids，在1和100μg/ kg的工作范围内线性校准，r> 0.991。两种类胡萝卜素的测定极限（LOD）和定量极限（LOQ）分别为苦味子苷B的5和10μg/ kg。类水果的类南瓜的回收率在85.3％至105.3％之间，变异系数在2.5％和12.8％之间。对水果和蔬菜提取物中干扰化合物的存在进行了评估，发现该干扰物质极少。由于线性行为，得出的结论是，前体离子的多个反应转变可用于分析目的，即用于痕量水平的水果和蔬菜提取物中的quassin，neosquasin和picrasinoside B的鉴定和定量。

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