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首页> 外文期刊>Analytica chimica acta >Enantioselective determination of triazole fungicide simeconazole in vegetables, fruits, and cereals using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) coupled to gas chromatography/tandem mass spectrometry
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Enantioselective determination of triazole fungicide simeconazole in vegetables, fruits, and cereals using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) coupled to gas chromatography/tandem mass spectrometry

机译:使用改良的QuEChERS(快速,简便,廉价,有效,坚固耐用和安全)与气相色谱/串联质谱联用,对蔬菜,水果和谷物中的三唑类杀菌剂西美康唑的对映选择性测定

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摘要

A rapid and effective method for enantioselective determination of simeconazole enantiomers in food products (cucumber, tomato, apple, pear, wheat and rice) has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (BGB-172) and a temperature program from 150°C (held for 1 min) and then raised at 10°Cmin~(-1) to 240°C (held for 10min). This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on the modification of QuEChERS (quick, easy, cheap, effective, rugged and safe) method. Co-extractives were removed with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. Gas chromatography/ion trap mass spectrometry (GC-ITMS) with electron ionization (EI) was then used for qualitative and quantitative determination of the simeconazole enantiomers. Two precursor-to-product ion transitions (m/z 121-101 and 195-153) with the best signal intensity were chosen to build the multiple-reaction monitoring (MRM) acquisition method. The limits of detection for each enantiomer of simeconazole in six food products ranged between 0.4 and 0.9μg kg~(-1), which were much lower than maximum residue levels (MRLs) established by Japan. The methodology was successfully applied for the enantioselective analysis of simeconazole enantiomers in real samples, indicating its efficacy in investigating the environmental stereochemistry of simeconazole in food matrix.
机译:已开发出一种快速有效的方法,用于食品(黄瓜,番茄,苹果,梨,小麦和大米)中西美康唑对映异构体的对映选择性测定。对映异构体通过毛细管气相色谱法(GC),使用商用手性色谱柱(BGB-172)进行拆分,温度程序从150°C(保持1分钟),然后在10°Cmin〜(-1)升至240°C C(保持10分钟)。这种对映选择性气相色谱分离方法基于QuEChERS(快速,简便,便宜,有效,坚固和安全)方法的改进,结合了净化/富集程序。使用石墨化炭黑/伯仲胺(GCB / PSA)固相萃取(SPE)柱(使用乙腈:甲苯(3:1,v / v)作为洗脱液)除去共提取物。然后将具有电子电离(EI)的气相色谱/离子阱质谱(GC-ITMS)用于西美康唑对映体的定性和定量测定。选择具有最佳信号强度的两个前体离子到产物离子的跃迁(m / z 121-101和195-153)来构建多反应监测(MRM)采集方法。六种食品中西美康唑的对映体的检出限在0.4至0.9μgkg〜(-1)之间,远低于日本确定的最大残留量(MRL)。该方法成功地用于实际样品中西美康唑对映异构体的对映选择性分析,表明其在研究食品基质中西美康唑的环境立体化学方面的功效。

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