Addison J B
J Assoc Off Anal Chem. 1982 Nov;65(6):1299-301.
A simplified method is described for the determination of chlorophacinone, 2-[(p-chlorophenyl)-phenylacetyl]-1,3-indandione, in homogenized mice. Chlorophacinone is extracted with acetonitrile. After Florisil cleanup, the extract is injected into a high pressure liquid chromatograph for reverse phase chromatography on a polar Lichrosorb NH2 (10 micron) column, with a mobile phase of acetonitrile-water (80 + 20). An injection containing 70 ng chlorophacinone produces 1/2 scale peaks at 254 nm with a full scale absorbance of 0.1 unit, an order of magnitude improvement over the sensitivity reported earlier with a 280 nm detector. Six homogenized mice samples and six spiked homogenized mice samples were quantitatively analyzed for trace levels of chlorophacinone by this method. Recoveries from spiked samples, as determined by peak height measurement, were greater than 95%. Mean retention time for the chlorophacinone peaks in all samples was 6.05 +/- 0.05 min. Chlorophacinone levels determined in homogenized whole mouse samples ranged from 0 to 63 ppm.
本文描述了一种测定匀浆小鼠中氯鼠酮（2-[(对氯苯基)-苯基乙酰基]-1,3-茚二酮）的简化方法。氯鼠酮用乙腈提取。经弗罗里硅土净化后，将提取物注入高压液相色谱仪，在极性的LiChrosorb NH2（10微米）柱上进行反相色谱分析，流动相为乙腈-水（80 + 20）。注入含70 ng氯鼠酮的溶液，在254 nm处产生半峰高的峰，满量程吸光度为0.1单位，比之前使用280 nm检测器报道的灵敏度提高了一个数量级。用该方法对六个匀浆小鼠样品和六个加标匀浆小鼠样品中的痕量氯鼠酮进行了定量分析。通过峰高测量确定，加标样品的回收率大于95%。所有样品中氯鼠酮峰的平均保留时间为6.05 +/- 0.05分钟。在匀浆的全小鼠样品中测定的氯鼠酮水平范围为0至63 ppm。
