Group "Analytical Chemistry of Contaminants", Department of Hydrogeology and Analytical Chemistry, University of Almeria, Spain.
Anal Bioanal Chem. 2011 Mar;399(8):2863-75. doi: 10.1007/s00216-011-4670-7. Epub 2011 Feb 1.
A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC-QqQ-MS/MS). A variety of methodologies has been evaluated, including solid-phase extraction (SPE), "dilute-and-shoot" (liquid-liquid extraction-based procedures), and QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods. The optimization and development process was carried out considering that the maximum residue level for aflatoxin M1 (AFM1) in milk in the European Union (EU) is set at 0.05 μg kg(-1), which is the lowest tolerance in the target compounds. The selected method consisted of an extraction by SPE using C18 as sorbent and methanol as elution solvent. The final determination was performed by UHPLC-QqQ-MS/MS. Matrix-matched standard calibration was used for quantification, obtaining recoveries in the range 60-120% with relative standard deviations <25%, at three spiking levels: 0.5, 10, and 50 μg kg(-1) (ten times lower for AFM1). Limits of quantification ranged from 0.20 to 0.67 μg kg(-1), which were always below or equal to the established tolerance levels by the EU. Finally, the selected method was applied to different types of milk.
一种快速多分析物方法已经被开发出来，用于通过超高效液相色谱-串联三重四极杆质谱（UHPLC-QqQ-MS/MS）同时测定牛奶中的农药和真菌毒素。评估了多种方法，包括固相萃取（SPE）、“稀释和进样”（基于液-液萃取的程序）和 QuEChERS（快速、简单、廉价、有效、耐用和安全）方法。优化和开发过程考虑到了欧盟（EU）中牛奶中黄曲霉毒素 M1（AFM1）的最大残留限量设定为 0.05μgkg-1，这是目标化合物中最低的容忍度。选择的方法包括使用 C18 作为吸附剂和甲醇作为洗脱溶剂的 SPE 提取。最终测定通过 UHPLC-QqQ-MS/MS 进行。采用基质匹配标准校准进行定量，在三个加标水平（0.5、10 和 50μgkg-1）下，回收率在 60-120%范围内，相对标准偏差<25%，AFM1 的加标水平低十倍。定量限范围为 0.20 至 0.67μgkg-1，始终低于或等于欧盟规定的容忍水平。最后，该方法应用于不同类型的牛奶。
