Consumer concerns over healthy diets are increasing as a result of the toxicity and persistence of pesticide residues in foodstuffs. Developing sensitive and high-throughput monitoring techniques for these trace residues is seen as an essential step in ensuring food safety. An automatic and sensitive multi-residue analytical method was developed and validated for the simultaneous determination of 230 compounds, including pesticides and their hazardous metabolites, in fermented soy products. The method included preparing the sample using on-line extraction and clean-up system based on accelerated solvent extraction (ASE), then determining the analytes using GC–MS/MS techniques. The homogenized samples (soy sauce, , and ) were automatically extracted at 80 °C and 10.3 MPa and at the same time, in situ cleaned by 300 mg of primary secondary amine (PSA) combined with 20 mg of hydroxylated multi-walled carbon nanotubes in an extraction cell. The method obtained excellent calibration linearity ( > 0.9220) and a satisfactory analysis of the targeted compounds, which were evaluated with matrix-matched calibration standards over the range of 5–500 μg L. The limit of detections (LODs) of analytes were in the range of 0.01–1.29 μg kg, 0.01–1.39 μg kg, and 0.01–1.34 μg kg in soy sauce, , and , respectively. The limit of quantifications (LOQs), which defined as the lowest spiking level, were set at 5.0 μg kg. The recoveries were within 70–120 % for over 95 % of the analytes, and the relative standard deviations (RSDs) were below 13.6 %. Moreover, a positive detection rate of 47 % were obtained when the proposed method was used on 15 real fermented soy products. These results suggested that the developed high-throughput method is highly feasible for monitoring of these target analytes in trace level.

中文翻译：

---

使用自动化一步加速溶剂萃取与 GC-MS/MS 相结合，改进了对三种发酵豆制品中 230 种农药残留的分析

由于食品中农药残留的毒性和持久性，消费者对健康饮食的担忧日益增加。开发针对这些痕量残留物的灵敏且高通量的监测技术被视为确保食品安全的重要步骤。开发并验证了一种自动、灵敏的多残留分析方法，可同时测定发酵豆制品中的 230 种化合物，包括农药及其有害代谢物。该方法包括使用基于加速溶剂萃取 (ASE) 的在线萃取和净化系统制备样品，然后使用 GC-MS/MS 技术测定分析物。均质后的样品（酱油、、、）在80℃、10.3MPa下自动提取，同时用300mg伯仲胺（PSA）结合20mg羟基化多壁碳纳米管进行原位清洗在提取室中。该方法获得了出色的校准线性 ( > 0.9220) 和对目标化合物的令人满意的分析，并在 5–500 µg L 范围内使用基质匹配的校准标准品进行评估。分析物的检测限 (LOD) 在酱油中的含量范围分别为 0.01–1.29 μg kg、0.01–1.39 μg kg 和 0.01–1.34 μg kg。定量限 (LOQ) 定义为最低加标水平，设定为 5.0 µg kg。超过 95% 的分析物的回收率在 70-120% 范围内，相对标准偏差 (RSD) 低于 13.6%。此外，该方法对15种真实发酵豆制品的阳性检出率为47%。这些结果表明，所开发的高通量方法对于痕量水平的这些目标分析物的监测非常可行。