Asadi Ali, Goudarzi Shokoufeh, Pakzad Saeedreza, Daraei Bahram, Firsukova Yana Artemovna, Mousavi Khaneghah Amin, Amirahmadi Maryam
Food and Drug Control Reference Laboratory, Food and Drug Administration, MOH and MOE, Tehran, Iran.
Food and Drug Laboratory Research Center, Food and Drug Administration, MOH MOE, Tehran, Iran.
Anal Methods. 2025 Jul 24;17(29):6034-6060. doi: 10.1039/d5ay00508f.
In this study, a modified "Quick, Easy, Cheap, Effective, Rugged, and Safe" (QuEChERS) sample preparation method, utilizing gas chromatography tandem mass spectrometry (GC-MS/MS), was employed for the simultaneous analysis of 222 pesticides in roasted coffee beans. The range and linearity of calibration curves, as well as the accuracy and intermediate precision, were assessed using spiked samples. Additionally, the Limits of Detection (LOD) and Quantitation (LOQ) were evaluated. The method has been linear in the 0.01-0.1 mg kg range. For most analytes, the mean recovery and Relative Standard Deviation (% RSD) were within the 70-120% range and under 20%, respectively. The mean recovery for all pesticides was 100.92 ± 10.69% at 0.015 mg kg, 107.61 ± 7.77% at 0.03 mg kg, and 96.63 ± 9.07% at 0.06 mg kg. Method validation demonstrated quantification capabilities for 222 analytes, with LOQs of 0.01 mg kg for 194 pesticides (87.4%), 0.015 mg kg for 26 compounds (11.7%), and 0.02 mg kg for the remaining 2 analytes (0.9%). Upon comparing the results with the requirements of SANTE/11312, it is evident that the method meets the necessary criteria to ensure the quality control of real samples. Out of 16 tested real coffee bean samples, three Arabica coffee bean samples contained residues of Flutriafol below the LOQ.
在本研究中，采用了一种改良的“快速、简便、廉价、高效、耐用、安全”（QuEChERS）样品制备方法，并结合气相色谱串联质谱法（GC-MS/MS），用于同时分析烘焙咖啡豆中的222种农药。通过加标样品评估校准曲线的范围和线性，以及准确度和中间精密度。此外，还评估了检测限（LOD）和定量限（LOQ）。该方法在0.01 - 0.1 mg/kg范围内呈线性。对于大多数分析物，平均回收率和相对标准偏差（%RSD）分别在70 - 120%范围内和20%以下。所有农药在0.015 mg/kg时的平均回收率为100.92 ± 10.69%，在0.03 mg/kg时为107.61 ± 7.77%，在0.06 mg/kg时为96.63 ± 9.07%。方法验证表明该方法对222种分析物具有定量能力，其中194种农药（87.4%）的LOQ为0.01 mg/kg，26种化合物（11.7%）的LOQ为0.015 mg/kg，其余2种分析物（0.9%）的LOQ为0.02 mg/kg。将结果与SANTE/11312的要求进行比较后发现，该方法符合确保实际样品质量控制的必要标准。在16个测试的真实咖啡豆样品中，有3个阿拉比卡咖啡豆样品中氟环唑的残留量低于LOQ。
