Fiddler W, Pensabene J W, Gates R A, Donoghue D J
Eastern Regional Research Center, Agricultural Research Service, U.S. Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, Pennsylvania 19038, USA.
J Agric Food Chem. 1999 Jan;47(1):206-11. doi: 10.1021/jf980436m.
The efficacy of supercritical fluid extraction (SFE) for the recovery of 16 common organochlorine pesticides (OCPs) from liquid whole eggs was investigated by employing supercritical carbon dioxide (SC-CO(2)) without the use of a solvent modifier to minimize interfering coextractives. The OCPs tested included aldrin; alpha-, beta-, delta-, and gamma-BHCs; p,p'-DDD, -DDE, and -DDT; dieldrin; endosulfans I, II, and sulfate; endrin; endrin aldehyde; heptachlor; and heptachlor epoxide. The SFE conditions were as follows: 10000 psi (680 bar), 40 degrees C, SC-CO(2) flow rate of 3.0 L/min with an extraction time of 40 min for a total of 120 L of CO(2). The OCPs were trapped off-line in an SPE cartridge containing Florisil and then eluted by an acetone/hexane mixture and analyzed by gas chromatography-electron capture detection (GC-ECD). Recovery studies were carried out on homogenized eggs fortified at the 0.05, 0.10, and 0.20 ppm levels. At the lowest level, 0.05 ppm, recoveries ranged from 81.8 to 108.3%, with CVs < 9.8%. All recoveries were significantly higher than those obtained by an AOAC/FDA solvent extraction method. Eggs containing incurred endosulfan I were also effectively extracted by SFE. This study suggests that the application of SFE for the extraction of OCPs from eggs will result in significant savings in analysis time and lower solvent use and disposal costs compared to conventional solvent extraction procedures.
采用超临界二氧化碳(SC-CO₂),不使用溶剂改性剂以尽量减少干扰性共提取物,研究了超临界流体萃取(SFE)从全蛋液中回收16种常见有机氯农药(OCPs)的效果。所测试的OCPs包括艾氏剂;α-、β-、δ-和γ-六六六;p,p'-滴滴滴、-滴滴伊和-滴滴涕;狄氏剂;硫丹Ⅰ、Ⅱ和硫酸盐;异狄氏剂;异狄氏剂醛;七氯;以及环氧七氯。SFE条件如下:10000磅力/平方英寸(680巴),40℃,SC-CO₂流速为3.0升/分钟,萃取时间为40分钟,共使用120升CO₂。OCPs离线捕集在装有弗罗里硅土的固相萃取柱中,然后用丙酮/己烷混合物洗脱,并通过气相色谱 - 电子捕获检测(GC-ECD)进行分析。对添加水平为0.05、0.10和0.20 ppm的匀浆鸡蛋进行了回收率研究。在最低水平0.05 ppm时,回收率范围为81.8%至108.3%,变异系数<9.8%。所有回收率均显著高于通过AOAC/FDA溶剂萃取法获得的回收率。含有硫丹Ⅰ的鸡蛋也能被SFE有效萃取。该研究表明,与传统溶剂萃取方法相比,应用SFE从鸡蛋中萃取OCPs将显著节省分析时间,并降低溶剂使用和处置成本。