Zacchei A G, Wishousky T I
J Pharm Sci. 1978 Feb;67(2):162-4. doi: 10.1002/jps.2600670210.
A specific and quantitative GLC method was developed for the determination of (2-cyclopentyl-6,7-dichloro-2-methyl-1-oxo-5-indanyloxy) acetic acid, a novel saluretic uricosuric agent, in biological fluids. The procedure involves the addition of an internal standard to the biological specimens followed by extraction of the acids into benzene at pH 1. The extracted acids, following back-extraction into base and reextraction into methylene chloride at an acidic pH, are converted to the respective methyl esters by reaction with ethereal diazomethane. The sensitivity of the method is such that 2 microgram of material can be detected per aliquot of plasma or urine. In the 2.5-50-microgram/ml range, recoveries were 98.1 +/- 9.6% (plasma, n = 157) and 99.3 +/- 6.4% (urine, n = 181). GLC-mass spectrometric techniques established analysis specificity.
已开发出一种特定的定量气相色谱法,用于测定生物体液中的新型促尿钠排泄尿酸排泄剂(2-环戊基-6,7-二氯-2-甲基-1-氧代-5-茚满氧基)乙酸。该方法包括向生物样本中加入内标物,然后在pH 1的条件下将酸萃取到苯中。萃取后的酸,经碱反萃取并在酸性pH下再萃取到二氯甲烷中,通过与乙醚重氮甲烷反应转化为相应的甲酯。该方法的灵敏度使得每份血浆或尿液等分试样中可检测到2微克物质。在2.5 - 50微克/毫升范围内,回收率分别为98.1±9.6%(血浆,n = 157)和99.3±6.4%(尿液,n = 181)。气相色谱 - 质谱技术确定了分析的特异性。