| 固相萃取/高效液相色谱法对火龙果中手性苯醚甲环唑的分离测定 |
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| 基金项目:海南省自然科学基金资助项目（20162034）；国家农产品质量安全风险评估重大专项（GJFP2017011） |
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| 中文摘要:建立了固相萃取/高效液相色谱测定火龙果中手性苯醚甲环唑的方法。火龙果样品经乙腈提取，石墨化炭黑/氨基固相萃取柱净化后进行测定。实验考察了不同手性色谱柱、流动相组成、流速及进样体积对分离的影响，通过优化分离成功拆分了苯醚甲环唑对映体。优化的色谱条件为：Chrialcel IF-3手性柱为色谱柱，正己烷-乙醇（92∶8，体积比）为流动相，流速为10 mL/min，进样量为60 μL。在上述条件下，4个对映体基本完全分离，分析时间不超过35 min。单个对映体在010~10 mg/L范围内呈良好的线性关系，检出限为0025 mg/L。分别添加04、28 mg/kg两个水平的外消旋苯醚甲环唑，测得4个对映体的平均回收率分别为837%~993%和864%~916%，相对标准偏差分别为13%~72%和14%~31%。该方法的分离时间较短，分离效果好，灵敏度高，适用于火龙果等水果中手性农药苯醚甲环唑含量的测定。 |
| 中文关键词:固相萃取 高效液相色谱法 火龙果 苯醚甲环唑对映体 手性农药 |
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| Separation and Determination of Chiral Difenoconazole in Dragon Fruit by Solid phase Extraction Coupled with High Performance Liquid Chromatography |
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| Abstract:A method was established for the determination of chiral difenoconazole in dragon fruit by solid phase extraction coupled with high performance liquid chromatography.The dragon fruit samples were extracted with acetonitrile，and purified with carbon black/amino solid phase extraction column.Effects of different chiral columns，mobile phase compositions，flow rates and injection volumes on chiral separation were investigated.The optimized chromatographic conditions were as follows：the chromatographic column：IF-3 chiral column，mobile phase：n hexane-ethanol（92∶8 by volume），injection volume：60 μL，flow rate：10 mL/min.Under the optimized conditions，the four difenoconazole enantiomers were basically achieved baseline separation，and the analysis time was less than 35 min.There existed a good linearity for each enantiomer in the range of 010-10 mg/L，with a detection limit of 0025 mg/L.The average recoveries for the chiral difenoconazole in dragon fruit at two spiked levels of 04 mg/kg and 28 mg/kg were in the ranges of 837%-993% and 864%-916%，with their RSDs of 13%-72% and 14%-31%，respectively.The developed method is rapid，accurate and sensitive，and is applicable for the determination of chiral difenoconazole residues in dragon fruit，etc. |
| Key Words:solid phase extraction(SPE) high performance liquid chromatography（HPLC） dragon fruit difenoconazole enantiomers chiral pesticides |
| 引用本文：张利强，邢淑莲，林丽云，林玲，叶剑芝，杨春亮.固相萃取/高效液相色谱法对火龙果中手性苯醚甲环唑的分离测定[J].分析测试学报,2018,37(8):945-949. |
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