Marine Environment Research Division, National Institute of Fisheries Science (NIFS), Busan 46083, Republic of Korea.
Marine Environment Research Division, National Institute of Fisheries Science (NIFS), Busan 46083, Republic of Korea.
Food Chem. 2016 Aug 15;205:1-8. doi: 10.1016/j.foodchem.2016.02.156. Epub 2016 Mar 3.
A rapid automated extraction and cleanup method using selective pressurized liquid extraction was developed and validated for 14 organochlorine pesticides in fish. The lipid-removal efficiencies achieved by adding alumina, Florisil, acid-treated silica gel, and silica gel to the extraction cell were determined and optimized. In the optimized method, fish (2-3g) was placed above alumina (30 g) in the extraction cell, then the sample was extracted using a 7:3 mixture of hexane and dichloromethane. The method was validated using certified reference materials (NIST SRM 1946 and 1974c), spiked fish, and four lipid-rich fish samples. The mean low- and high-concentration spike recoveries were 91% and 93% with RSD<20%, respectively. Measured concentrations of target OCPs showed good agreement with the certified concentrations in certified reference materials. It suggests the good accuracy and precision of the SPLE method. The proposed method met the most important requirements of an extraction and cleanup procedure, including having a short preparation (cleanup and concentration) time and minimal sample contamination and being able to be automated.
建立并验证了一种用于鱼中 14 种有机氯农药的快速自动化萃取净化方法，该方法采用选择性加压液体萃取。通过向萃取池添加氧化铝、弗罗里硅土、酸处理硅胶和硅胶，确定并优化了去除脂质的效率。在优化的方法中，将鱼（2-3g）置于萃取池中的氧化铝（30g）上方，然后使用 7：3 的正己烷和二氯甲烷混合物萃取样品。使用认证参考物质（NIST SRM 1946 和 1974c）、加标鱼和四种富含脂质的鱼样品对方法进行了验证。低浓度和高浓度加标回收率的平均值分别为 91%和 93%，相对标准偏差<20%。目标 OCPs 的实测浓度与认证参考物质中的认证浓度具有良好的一致性。这表明 SPLE 方法具有良好的准确性和精密度。所提出的方法满足萃取和净化程序的最重要要求，包括具有短的制备（净化和浓缩）时间、最小的样品污染以及能够自动化。
