An analytical method for the accurate determination of carbamate pesticides, carbaryl, carbendazim, and carbofuran, in vegetables was established based on the isotope dilution liquid chromatography/tandem mass spectrometry (ID-LC/MS/MS) technique as a candidate reference method. For sample clean-up, a Carb/LC-NH2 solid-phase extraction (SPE) cartridge was employed to ensure an efficient recovery and color removal from the vegetable samples. Isotope analogues, 13 C 6 -carbaryl, carbendazim- d 4 , and 13 C 6 -carbofuran, were used as internal standards, respectively. This method was validated by measuring samples fortified with the three target analytes into vegetable samples and prepared homogeneous Korean cabbage powder samples in this laboratory. All results of the measured values agreed with the fortified values within their uncertainties. Repeatability and reproducibility of the method were both approximately 2%. As commercially available CRM contains only carbendazim, its content was analyzed by the developed method. The measured value of carbendazim in CRM was (0.0724 ± 0.0013) mg/kg agreeing with the certified value (0.074 ± 0.004) mg/kg. These validation data indicate the developed ID-LC/MS/MS method is reproducible, repeatable and reliable to be as a candidate reference method for accurate determination of carbamate pesticides in vegetables.

中文翻译：

---

同位素稀释液相色谱/串联质谱法准确测定蔬菜中的甲萘威、克百威和多菌灵

以同位素稀释液相色谱/串联质谱 (ID-LC/MS/MS) 技术为候选参考方法，建立了一种准确测定蔬菜中氨基甲酸酯类农药、甲萘威、多菌灵和呋喃丹的分析方法。对于样品净化，采用 Carb/LC-NH2 固相萃取 (SPE) 小柱以确保植物样品的有效回收和颜色去除。同位素类似物， 13 C 6 -carbaryl、多菌灵-d 4 和 13 C 6 -carbofuran 分别用作内标。该方法通过测量添加了三种目标分析物的样品进入蔬菜样品并在该实验室制备的均质韩国卷心菜粉样品得到验证。测量值的所有结果在其不确定度范围内与强化值一致。该方法的重复性和再现性均约为 2%。由于市售的 CRM 仅包含多菌灵，因此通过开发的方法对其含量进行了分析。CRM中多菌灵的测定值为（0.0724±0.0013）mg/kg，与认证值（0.074±0.004）mg/kg一致。这些验证数据表明，开发的 ID-LC/MS/MS 方法具有重现性、可重复性和可靠性，可作为准确测定蔬菜中氨基甲酸酯类农药的候选参考方法。