College of Biology and Environmental Engineering, Zhejiang Shuren University, Hangzhou, China, 310015.
College of Chemical Engineering, Zhejiang University of Technology, Hangzhou, China, 310014.
Anal Methods. 2022 Jan 20;14(3):250-258. doi: 10.1039/d1ay01764k.
This study established a detection method based on accelerated solvent extraction-liquid chromatography-mass spectrometry for determining residues of 3 chloramphenicols, 8 macrolides, 18 sulfonamides, 4 nitroimidazoles, 15 insecticides, and 22 fungicides in poultry feathers. The extraction solvent, methanol, was used for a static extraction time of 5 min, and repeated three times. Fifty milligrams of adsorbents C18/PSA (1 : 1, W/W) were added to the extraction cell to achieve simultaneous extraction and purification. The extraction efficiency of three solvents, methanol, acetonitrile and ethyl acetate, was investigated. An orthogonal experimental design was used to explore the optimal combination of extraction temperature, static extraction time, number of extraction cycles, and adsorbent ratio for accelerated solvent extraction. After the optimal ratio was determined, the dosage of adsorbents was optimized. The extracted sample solution was concentrated by blowing nitrogen, redissolved, passed through a 0.22 μm PTFE membrane filter, then injected for instrumental analysis. The validation results showed that the recovery of the proposed method was 60.4-107.6%, the limit of detection 0.2-3.0 μg kg, and the limit of quantification 0.5-8.3 μg kg. This quantitative multi-residue detection method was able to determine the residues of 70 target compounds in poultry feathers.
本研究建立了一种基于加速溶剂萃取-液相色谱-质谱法测定禽毛中 3 种氯霉素、8 种大环内酯类、18 种磺胺类、4 种硝基咪唑类、15 种杀虫剂和 22 种杀菌剂残留的检测方法。提取溶剂为甲醇，静态提取时间为 5 min，重复 3 次。向提取池中加入 50mg 的 C18/PSA（1:1，W/W）吸附剂，实现同时提取和净化。考察了甲醇、乙腈和乙酸乙酯三种溶剂的提取效率。采用正交实验设计，探讨了加速溶剂萃取中提取温度、静态提取时间、提取循环次数和吸附剂比例的最佳组合。确定最佳比例后，优化了吸附剂用量。提取样品溶液经氮气吹脱浓缩、复溶后，通过 0.22 μm PTFE 膜过滤器过滤，然后进行仪器分析。验证结果表明，该方法的回收率为 60.4%-107.6%，检出限为 0.2-3.0μg/kg，定量限为 0.5-8.3μg/kg。该定量多残留检测方法能够测定禽毛中 70 种目标化合物的残留。
