Background At present, plant growth regulators (PGRs) are widely used in agricultural and forestry production. PGRs, like traditional pesticides, have certain toxicities. Naively excessively applying them will cause the acute and chronic poisoning of humans and animals and potentially harm human health. Objective In order to assess, prevent, and control the residues of PGRs in fruits and vegetables, a set of quick, easy, cheap, effective, rugged, and safe (QuEChERS) analytical methods that simultaneously detect multiple PGR residues are urgently needed for quality and safety inspection of agricultural product. Methods In this study, grapes (representative of fruits) and cabbages (representative of vegetables) were used as the detected objects. The 30 commercial product residues of PGRs were detected in both with an ultra-high performance liquid chromatography (UHPLC)-tandem mass spectrometry (MS/MS) method, based on optimized chromatographic, MS, and preparation conditions (extraction solvent and cleanup conditions). Grape and cabbage samples were extracted with acetonitrile containing 5% (v/v) acetic acid, dehydrated using a salt package, purified using the QuEChERS method, ionized using electrospray ionization under positive and negative ion switching mode, detected using multi-reaction monitoring, and quantification using an external standard method of matrix matching standard curve. Results Methanol was selected as the strong elution phase. A methanol-0.1% formic acid-5 mmol/L ammonium acetate solution was selected as the best mobile phase. The optimal extraction solvent was acetonitrile containing 5% acetic acid. Primary secondary amine cleanup could met the determination requirements of PGR residues. The developed method for determination of 30 commercial products of PGR, such as betaine, showed excellent linearity in 1–500, 10–1000, ∼500, ∼2000, and 100–10 000 μg/kg (R ≥ 0.98). At the 0.001 (0.01), 0.05, 0.20, and 1.00 mg/kg additive concentrations, the average addition standard recovery of 30 commercial products of PGR were 61–132% with the relative standard deviations of 1–14% and the LOQs were confirmed to be 1.0–100 μg/kg through the actual addition values of samples. Conclusion The set of optimized QuEChERS UHPLC-MS/MS methods simultaneously detect residues of PGRs in fruits and vegetables with one-time sample preparation for high-throughput, rapid quantitative screening, and confirmation. The methods cover a wide range of PGRs with simple and convenient preparation and small amounts of solvent, and can provide technical support for the supervision of PGR residues in fruits and vegetables. Highlights The optimizations of extraction solvent screening, different ratios of various purification packages in the QuEChERS method, and UPLC-MS conditions were conducted and the precision, sensitivity, and recovery rates of the methods were investigated in order to establish a QuEChERS UPLC-MS/MS method for simultaneously detecting 30 kinds of PGR residues in fruits and vegetables. The methods allow high-throughput determination of multiple PGR residues in fruits and vegetables and can also provide technical references for related compound residue detection of other matrixes.

中文翻译：

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使用优化的 QuEChERS 样品制备和 UHPLC-MS/MS 方法同时检测卷心菜和葡萄中的多种植物生长调节剂残留

背景技术目前，植物生长调节剂（PGRs）广泛应用于农业和林业生产。PGR 与传统农药一样，具有一定的毒性。天真地过度使用它们会导致人和动物的急性和慢性中毒，并可能危害人类健康。目的 为评估、预防和控制果蔬中的 PGRs 残留，急需一套快速、简便、廉价、有效、耐用、安全（QuEChERS）同时检测多种 PGRs 残留的分析方法，以提高质量。农产品安全检验。方法本研究以葡萄（代表水果）和卷心菜（代表蔬菜）为检测对象。基于优化的色谱、质谱和制备条件（萃取溶剂和净化条件），采用超高效液相色谱 (UHPLC)-串联质谱 (MS/MS) 方法检测了 30 种 PGRs 商业产品残留. 葡萄和卷心菜样品用含有 5% (v/v) 乙酸的乙腈提取，使用盐包脱水，使用 QuEChERS 方法纯化，在正负离子切换模式下使用电喷雾电离进行电离，使用多反应监测进行检测，并采用基质匹配标准曲线的外标法定量。结果选择甲醇作为强洗脱相。选择甲醇-0.1% 甲酸-5 mmol/L 乙酸铵溶液作为最佳流动相。最佳萃取溶剂为含 5% 乙酸的乙腈。一级仲胺净化可满足PGR残留量的测定要求。所开发的测定 30 种 PGR 商业产品（如甜菜碱）的方法在 1-500、10-1000、~500、~2000 和 100-10 000 μg/kg (R ≥ 0.98) 范围内表现出优异的线性。在 0.001 (0.01)、0.05、0.20 和 1.00 mg/kg 添加剂浓度下，30 种 PGR 商业产品的平均添加标准回收率为 61-132%，相对标准偏差为 1-14%，并确认了 LOQ 1.0~100 μg/kg，以样品的实际添加值为准。结论 这套优化的 QuEChERS UHPLC-MS/MS 方法可同时检测水果和蔬菜中的 PGRs 残留，一次性样品制备，用于高通量、快速定量筛选，和确认。该方法覆盖范围广，制备简便，溶剂用量少，可为果蔬PGR残留监管提供技术支持。亮点 对提取溶剂筛选、QuEChERS 方法中各种纯化包的不同比例、UPLC-MS 条件进行了优化，并研究了方法的精密度、灵敏度和回收率，以建立 QuEChERS UPLC-MS/ MS法同时检测果蔬中30种PGR残留量 该方法可实现果蔬中多种PGR残留的高通量测定，也可为其他基质的相关化合物残留检测提供技术参考。该方法覆盖范围广，制备简便，溶剂用量少，可为果蔬PGR残留监管提供技术支持。亮点 对提取溶剂筛选、QuEChERS 方法中各种纯化包的不同比例、UPLC-MS 条件进行了优化，并研究了方法的精密度、灵敏度和回收率，以建立 QuEChERS UPLC-MS/ MS法同时检测果蔬中30种PGR残留量 该方法可实现果蔬中多种PGR残留的高通量测定，也可为其他基质的相关化合物残留检测提供技术参考。该方法覆盖范围广，制备简便，溶剂用量少，可为果蔬PGR残留监管提供技术支持。亮点 对提取溶剂筛选、QuEChERS 方法中各种纯化包的不同比例、UPLC-MS 条件进行了优化，并研究了方法的精密度、灵敏度和回收率，以建立 QuEChERS UPLC-MS/ MS法同时检测果蔬中30种PGR残留量 该方法可实现果蔬中多种PGR残留的高通量测定，也可为其他基质的相关化合物残留检测提供技术参考。