Zhuang Wenshan, McKague Bruce, Reeve Douglas, Carey John
Department of Chemical Engineering and Applied Chemistry, University of Toronto, 200 College St., Toronto, ON, Canada M5S 3E5.
Chemosphere. 2004 Jan;54(4):467-80. doi: 10.1016/j.chemosphere.2003.08.024.
Optimal conditions for extraction methods using an accelerated solvent extractor (ASE) and a Polytron homogenizer were established for quantification of (crude) lipids and extractable organochlorine (EOCl) in fish. The two methods, an ASE consecutive extraction at 55 and 100 degrees C for ground, freeze-dried filets, and a Polytron extraction at room temperature with four repetitions for ground, wet filets and with two repetitions for wet fish livers were evaluated in terms of reproducibility and comparability. With respect to lipid measurement, the two methods have comparable reproducibility and the experimental errors are relatively small compared to natural variations of fish to fish within a sampling site. For EOCl measurement, the relative standard deviation tends to increase with decreasing levels of EOCl in specimens. An important factor for the relative standard deviation of measurements of analytes present at trace levels in fish matrices is sampling error in taking aliquots. Statistical analysis using a paired comparison design showed that measurement values (crude lipids or EOCl) obtained from these two extraction methods are, in general, not equivalent. There is a good correlation between the two methods for lipid measurement; whereas for EOCl measurements, high degrees of correlation exist within the exposed fish group, but not in the reference group.
建立了使用加速溶剂萃取仪(ASE)和Polytron匀浆器的萃取方法的最佳条件,用于定量鱼类中的(粗)脂质和可萃取有机氯(EOCl)。对两种方法进行了评估,一种是在55和100摄氏度下对研磨后的冻干鱼片进行ASE连续萃取,另一种是在室温下对研磨后的湿鱼片进行四次重复的Polytron萃取,对湿鱼肝进行两次重复萃取,评估指标为重现性和可比性。在脂质测量方面,两种方法具有可比的重现性,与采样点内鱼与鱼之间的自然差异相比,实验误差相对较小。对于EOCl测量,相对标准偏差往往随着标本中EOCl水平的降低而增加。鱼类基质中痕量水平分析物测量相对标准偏差的一个重要因素是取等分试样时的采样误差。使用配对比较设计的统计分析表明,从这两种萃取方法获得的测量值(粗脂质或EOCl)通常不相等。两种方法在脂质测量方面具有良好的相关性;而对于EOCl测量,在暴露鱼类组内存在高度相关性,但在参考组中不存在。