改进的QuEChERS-超高效液相色谱-串联质谱法检测4种热带水果中的17种植物生长调节剂残留

    Determination of seventeen plant growth regulator residues in four tropical fruits by a modified QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

    • 摘要: 建立了一种基于超高效液相色谱-串联质谱(UPLC-MS/MS)技术的方法,用于同时测定杨桃(Averrhoa carambola)、番木瓜(Carica papaya)、鳄梨(Persea americana)和黄皮(Clausena lansium)果实中的17种植物生长调节剂(PGRs)。采用QuEChERS法进行果实样品前处理,并针对提取盐、提取方式、提取溶剂量、提取时间、净化材料等前处理条件进行了优化,最终确定了以4 g MgSO4 + 1 g NaCl + 1 g Na3Cit·2H2O + 0.5 g Na2HCit·1.5H2O为提取盐和25 mL乙腈为提取溶剂对10 g样品振荡提取10 min,采用150 mg MgSO4和30 mg C18作为净化材料对水果提取液进行净化。目标物采用多反应监测(sMRM)模式进行定性,并采用基质匹配外标法进行定量。该方法根据欧盟农药残留分析方法验证指导原则(SANTE/11312/2021(V2))进行了方法学考察。17种PGRs在0.05 ~ 20 µg/kg或0.5 ~ 20 µg/kg线性关系良好,相关系数均大于0.999。在低、中、高水平加标浓度下的回收率结果表明:日内和日间的回收率均在80% ~ 120%,相对标准偏差均低于20%。结果证实了本研究所建立的方法适用于4种水果中17种PGRs的同时分析。以上方法被用于检测海口市场购买的水果样品,最终检测出13种PGRs残留,其中,抗倒酯和5-硝基愈创木酚钠在4种水果样品中均有检出。本研究将为热带水果中PGRs多残留分析方法的建立提供技术参考。

       

      Abstract: A method based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) technology was developed for the rapid and simultaneous detection of 17 plant growth regulators (PGRs) in the fruits of carambola (Averrhoa carambola), papaya (Carica papaya), avocado (Persea americana), and wampee (Clausena lansium). The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was adopted for the pre-treatment of fruit samples in this study, and the pre-treatment factors, such as the phase-out salt, extraction method, extraction solvent, extraction time, and purification materials were optimized. The final pre-treatment method was determined to use 25 mL of acetonitrile for the extraction of 10 g samples by votexing for 10 min, followed by the phasing-out with the mixed salts including 4 g MgSO4 + 1 g NaCl + 1 g Na3Cit·2H2O + 0.5 g Na2HCit·1.5H2O , Then 150 mg of MgSO4 and 30 mg of C18 was used as purification materials to purify the extracts. The 17 target PGRs were detected using multi-reaction monitoring (sMRM) mode and quantified with the matrix-matched external standard method. The method was validated according to the European guideline of SANTE/11312/2021(V2). The linearity for the 17 PGRs was excellent in the range of 0.05 to 20 μg/kg or 0.5 to 20 μg/kg, with correlation coefficients all greater than 0.999. The results at low, medium, and high spiked levels showed that the intra-day and inter-day recovery rates were 80% to 120% with relative standard deviations all below 20%. The results confirmed that the proposed method was suitable for the routine detection of these pesticides in the four fruit samples. The established method was used to detect the fruit samples purchased from the local markets in Haikou city, China. The residues of 13 PGRs were detected, among which trinexapac-ethyl and 5-nitroguaiacol sodium salt were detected in the samples of all four fruits. This study provides technical reference for the establishment of multi residue analysis methods for PGRs in tropical fruits.

       

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