| 固相萃取/液相色谱-串联质谱法测定水果蔬菜中双胍辛胺的残留量 |
| 点此下载全文 |
|
| 基金项目:海关总署科研项目（2020HK206）；支撑“一带一路”贸易便利化的认证认可关键技术研究与应用（二期）项目（2018YFF0215600） |
|
| 中文摘要:建立了测定沃柑、菠萝蜜、苹果、葡萄、生菜、黄瓜、西红柿、芦笋等水果蔬菜中双胍辛胺残留量的固相萃取/液相色谱－串联质谱方法。试样用0.2%乙酸水提取，二氯甲烷萃取杂质，提取液经WCX固相萃取柱净化，10%甲酸乙腈洗脱，氮吹至近干后以0.2%甲酸水复溶。采用甲醇和0.2%甲酸水为流动相，经Eclipse Plus C18（2.1 mm × 100 mm，1.8 μm）分离，在电喷雾离子源正离子模式下采用双胍辛胺的双电荷加合母离子m/z?178.8及其子离子m/z?100.0和187.0进行多反应监测（MRM）扫描，基质加标曲线进行定量。结果表明，双胍辛胺在0.005～0.160 mg/kg范围内线性关系良好，相关系数r?≥ 0.995；0.010、0.020、0.050 mg/kg加标水平下的平均回收率为88.5%～109%，相对标准偏差（RSD，n?= 6）为2.1%～8.8%；方法检出限为0.005 mg/kg，定量下限为0.010 mg/kg。该方法快速、准确、灵敏，适用于水果蔬菜中双胍辛胺残留量的测定。 |
| 中文关键词:双胍辛胺 ?双胍三辛烷基苯磺酸盐 ?沃柑 ?固相萃取 ?液相色谱－串联质谱 |
| |
| Determination of Iminoctadine Residues in Fruits and Vegetables by Solid Phase Extraction and Liquid Chromatography－ Tandem Mass Spectrometry |
|
|
| Abstract:A solid phase extraction and liquid chromatography－tandem mass spectrometry was developed for the determination of iminoctadine residues in fruits and vegetables including citrus，jackfruit，apple，grape，lettuce，cucumber，tomato and asparagu．Samples were extracted with 0.2% acetic acid，and preliminarily purified with dichloromethane. The extract solution was purified using a WCX solid phase extraction column，and the target compound was eluted with 10% formic acid acetonitrile．The eluent was blown to near dryness with nitrogen，and then redissolved with 0.2% formic water．The compound was separated on a C18 column with methanol and 0.2% formic acid water as mobile phases．The double charges additive ion m/z?178.8 and its daughter ions?m/z?100.0 and 187.0 from iminoctadine were selected for the multi reaction monitoring（MRM） scanning under the positive ion mode of electrospray ion source（ESI+）．The iminoctadine in the samples was quantified by the calibration curve of matrix addition standard．The correlation coefficients（r） were not less than 0.995，which indicated that the linear dependence of iminoctadine was good in the range of 0.005－0.160 mg/kg．The limits of detection（LOD） and quantitation（LOQ） for iminoctadine were 0.005 mg/kg and 0.010 mg/kg，respectively．The average recoveries at spiked levels of 0.010，0.020 and 0.050 mg/kg ranged from 88.5% to 109%，with the relative standard deviations（RSDs，n?= 6） of 2.1%－8.8%．With the advantages of rapidness，accuracy and sensitivity，this method is suitable for the determination of iminoctadine in fruits and vegetables． |
| Key Words:iminoctadine ?iminoctadine tris（albesilate） ?citrus ?solid phase extraction ?liquid chromatography－tandem mass spectrometry |
| 引用本文：秦富，汪文龙，司露露，蔡翔宇，梁宇，苏华，韦涛.固相萃取/液相色谱-串联质谱法测定水果蔬菜中双胍辛胺的残留量[J].分析测试学报,2022,41(5):768-773. |
| 摘要点击次数: 980 |
| 全文下载次数: 892 |
| 查看全文 下载PDF阅读器 |
|
|
