QuEChERS-液相色谱-串联质谱法测定大米中14种琥珀酸脱氢酶抑制剂类杀菌剂残留量

Determination of 14 kinds of succinate dehydrogenase inhibitor fungicides in rice by QuEChERS-liquid chromatography-tandem mass spectrometry

中文关键词:  QuEChERS  液相色谱-串联质谱法  琥珀酸脱氢酶抑制剂类杀菌剂  多级反应监测触发增强子离子扫描模式  大米

英文关键词:QuEChERS  liquid chromatography-tandem mass spectrometry  succinate dehydrogenase inhibitor fungicides  multiple reaction monitoring-information dependent acquisition-enhanced product ion  rice

中文摘要:

      目的 建立QuEChERS-液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)测定大米中14种琥珀酸脱氢酶抑制剂(succinate dehydrogenase inhibitor, SDHI)类杀菌剂(氟吡菌酰胺、吡噻菌胺、萎锈灵、联苯吡菌胺、吡唑萘菌胺、氟唑环菌胺、氟唑菌苯胺、氟苯吡菌胺、呋吡菌胺、氟酰胺、氟啶酰菌胺、氟吡菌酰胺-苯甲酰胺、甲呋酰胺、噻呋酰胺)残留的分析方法。方法 样品经乙腈提取后, 用QuEChERS法净化浓缩, Symmetry C18色谱柱(150 mm×2.1 mm, 3.5 μm)分离, 在碰撞能量为(35±15) eV条件下, 采用多级反应监测触发增强子离子扫描模式(multiple reaction monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI)进行定性分析并建立增强子离子扫描谱库, LC-MS/MS外标法定量。结果 该方法具有较高的灵敏度, 14种SDHI类杀菌剂的定量限为0.10 μg/kg; 在0.05~5.00 μg/L质量浓度范围, 线性相关系数大于等于0.99936, 平均回收率在82.5%~108.3%之间, 相对标准偏差在2.1%~11.9%之间。结论 该方法前处理过程简便、灵敏度高, 通过谱库比对, 定性准确性大大提高, 适用于大米中SDHI类杀菌剂残留的定性定量分析。

英文摘要:

      Objective To establish a method for the determination of 14 kinds of succinate dehydrogenase inhibitor (SDHI) fungicides (fluopyram, penthiopyrad, carboxin, bixafen, isopyrazam, sedaxane, penflufen, fluxapyroxad, furametpyr, flutolanil, fluopicolide, fluopyram-benzamide, fenfuram, thifluzamide) in rice by QuEChERS-liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods After extracted by acetonitrile, the samples were purified and concentrated by QuEChERS method, separated by Symmetry C18 column (150 mm×2.1 mm, 3.5 μm), under the condition of collision energy of (35±15) eV, qualitative and quantitative analysis were carried out using predictive multiple reaction monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) scanning, and the enhanced product ion spectrum library was established and quantified by LC-MS/MS with external standard method. Results The method had high sensitivity, the limits of quantification of 14 kinds of SDHI fungicides were 0.10 μg/kg, and the linear correlation coefficients were greater than or equal to 0.99936 respectively in the mass concentration range of 0.05?5.00 μg/L. The average recoveries were 82.5% to 108.3%, and the relative standard deviations were 2.1%?11.9%. Conclusion This method is pretreatment process simple and sensitive, through the comparison of spectrum library, and greatly improves the qualitative accuracy, this method suitable for qualitative and quantitative analysis of SDHI bactericide residues in rice.