| 苏丽梅,何京明,黄秋琳,唐念念,李灿玲,韦思羽,何小娟,陈泽龙,刘守廷.QuEChERS-液相色谱-串联质谱法测定沃柑中噻唑锌、氟吡菌酰胺、亚胺唑、毒菌酚残留量[J].中国南方果树,2025,54(3): |
| QuEChERS-液相色谱-串联质谱法测定沃柑中噻唑锌、氟吡菌酰胺、亚胺唑、毒菌酚残留量 |
| Determination of zinc thiazole, fluopyramandand, imibenconazole and hexachlorophene residues in orah by QuEChERS-Liquid chromatography-Tandem mass spectrometry |
| 投稿时间：2024-05-28 修订日期：2024-07-24 |
| DOI： |
| 中文关键词: 沃柑 液相色谱-串联质谱法 噻唑锌 氟吡菌酰胺 亚胺唑 毒菌酚 |
| 英文关键词:orah liquid chromatography-mass spectrometry zinc thiazole fluopyramandand imibenconazole hexachlorophene |
| 基金项目:广西壮族自治区南宁市科学研究与技术开发计划项目《沃柑中杀菌剂类农药残留关键检测技术的研究》（20212149）；广西壮族自治区重点研发项目《柑橘杀虫剂和杀菌剂农药残留快速检测技术研究及示范应用》（桂科AB23075085） |
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| 中文摘要: |
| 建立了超高效液相色谱-串联质谱法同时测定沃柑中噻唑锌、氟吡菌酰胺、亚胺唑、毒菌酚残留量的分析方法。样品在37 ℃经1.0 mol/L硫代硫酸钠溶液转化30 min，用1.0 mol/L盐酸溶液调节pH值为3，以0.5％甲酸乙腈作提取溶剂，每毫升提取液加入25 mg C18和2.5 mg carbon S吸附剂净化，然后用C18-AQ高效液相色谱柱在电喷雾模式下进行多重反应监测(MRM)分析，以基质匹配标准曲线外标法定量。噻唑锌、氟吡菌酰胺、亚胺唑、毒菌酚在0.002 mg/L～0.5 mg/L范围浓度与峰面积呈良好的线性关系，相关系数(r)均≥0.998。结果表明，该方法噻唑锌、氟吡菌酰胺、亚胺唑、毒菌酚定量限分别为0.004 mg·kg-1、0.003 mg·kg-1、0.006 mg·kg-1和0.002 mg·kg-1，加标回收率分别为73.17％±12.52％、93.85％±22.95％、89.70％±19.78％和98.68％±20.48％，精密度RSD分别为9.14％、8.50％、8.71％和8.01％（n=7）。 |
| 英文摘要: |
| An analytical method was developed to simultaneously determine the residues of zinc thiazole, fluopyramand, imibenconazoleand hexachlorophene residues in orah using ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The samples were transformed at 37 °C for 30 minutes using 1.0 mol/L sodium thiosulfate solution, adjusted to a pH of approximately 3 with 1.0 mol/L hydrochloric acid solution, and extracted with 0.5% formic acid acetonitrile. The extract was purified by adding 25 mg of C18 and 2.5 mg of carbon S adsorbents per milliliter, followed by analysis on a C18-AQ high-performance liquid chromatography column under electrospray ionization mode using multiple reaction monitoring (MRM). Quantification was performed using matrix-matched calibration curves and external standards. The method exhibited good linearity for zinc thiazole, fluopyramand, imibenconazole, and hexachlorophene within the range of 0.002 mg/L to 0.5 mg/L, with correlation coefficients (r) all ≥0.998. The limits of quantification (LOQs) for zinc thiazole, fluopyramand, imibenconazole, and hexachlorophene were 0.004 mg/kg, 0.003 mg/kg, 0.006 mg/kg, and 0.002 mg/kg, respectively. The spiked recovery rates ranged 73.17％±12.52％for zinc thiazole, 93.85％±22.95％for fluopyramand,89.70％±19.78％for imibenconazole, and 98.68％±20.48％ for hexachlorophene, with relative standard deviations (RSDs) of 9.14%, 8.50%, 8.71%, and 8.01%, respectively (n=7). |
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