Sagratini Gianni, Mañes Jordi, Giardiná Dario, Damiani Pietro, Picó Yolanda
Dipartimento di Scienze Chimiche, Facoltà di Farmacia, Università di Camerino, via S.Agostino 1, 62032 Camerino, Italy.
J Chromatogr A. 2007 Apr 20;1147(2):135-43. doi: 10.1016/j.chroma.2007.02.066. Epub 2007 Feb 24.
A new analysis method to detect carbamates and phenylurea pesticide residues in fruit juices was developed using solid-phase microextraction (SPME) coupled with liquid chromatography-single quadrupole mass spectrometry (LC/MS) and liquid chromatography-quadrupole ion trap mass spectrometry (LC/QIT-MS). The pesticide residues present in watery matrices as fruit juices were extracted using three types of fibers: 50-microm Carbowax/templated resin (CW/TPR), 60-mum poly(dimethylsiloxane)/divinylbenzene (PDMS/DVB) and 85-microm polyacrylate. The different extraction conditions were evaluated choosing as the best parameters 90 min (time), 20 degrees C (temperature) and 1 ml (volume). After extraction, the desorption (in a static mode) was performed in the specific interface chamber SPME/HPLC, previously filled with 70% methanol and 30% water. The best recoveries, evaluated at two fortification levels (0.2 and 0.5 mg kg(-1)) in fruit juices, were obtained using PDMS/DVB and CW/TPR fibers, and ranged from 25 to 82% (monolinuron, diuron and diethofencarb), with relative standard deviations (RSDs) from 1 to 17%. All the limits of quantification (LOQs) were in the range of 0.005-0.05 microg ml(-1) and, in any case, equal to, or lower than, maximum residue limits (MRLs) established by Italian and Spanish legislations. The mass spectrometry analyses were carried out using an electrospray ionization (ESI) source operating in the positive mode both for single quadrupole and for QIT mass analysers, operating in selected ion monitoring (SIM) and in multiple reaction monitoring (MRM) modes, respectively. The proposed new method can be applied to the determination of selected pesticides in real samples of fruit juices.
开发了一种新的分析方法，用于检测果汁中的氨基甲酸酯类和苯基脲类农药残留，该方法采用固相微萃取（SPME）结合液相色谱 - 单四极杆质谱（LC/MS）和液相色谱 - 四极杆离子阱质谱（LC/QIT-MS）。使用三种类型的纤维萃取果汁等水性基质中的农药残留：50微米的聚乙二醇/模板树脂（CW/TPR）、60微米的聚二甲基硅氧烷/二乙烯基苯（PDMS/DVB）和85微米的聚丙烯酸酯。评估了不同的萃取条件，选择90分钟（时间）、20℃（温度）和1毫升（体积）作为最佳参数。萃取后，在预先充满70%甲醇和30%水的特定接口室SPME/HPLC中进行（静态模式下的）解吸。在果汁中两个加标水平（0.2和0.5毫克/千克）下评估，使用PDMS/DVB和CW/TPR纤维获得了最佳回收率，范围为25%至82%（灭草隆、敌草隆和乙霉威），相对标准偏差（RSD）为1%至17%。所有定量限（LOQ）在0.005 - 0.05微克/毫升范围内，并且在任何情况下均等于或低于意大利和西班牙法规规定的最大残留限量（MRL）。质谱分析使用电喷雾电离（ESI）源，单四极杆和QIT质量分析仪均在正模式下运行，分别在选择离子监测（SIM）和多反应监测（MRM）模式下操作。所提出的新方法可应用于实际果汁样品中选定农药的测定。
