摘要目的 建立尿样中1-羟基-2-丁酮的气相色谱测定方法.方法 尿样经盐酸酸化后冷冻保存,自然解冻后,取2.0 ml尿样经C18固相柱萃取,2.0 ml甲醇洗脱,取洗脱液约1.0 ml于进样瓶中,用带火焰离子化检测器(FID)的气相色谱仪进行检测,外标法定量.结果 该方法线性范围为0.986~32.880μg/ml,r=0.999 7,方法检出限为0.13 μg/ml;样品加标回收率为88.1%~92.2%,批内、批间精密度分别为1.4~2.1%、2.3%~3.2%.结论该方法灵敏度高、样品处理简单,各项技术指标均能满足测定方法要求.
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abstractsObjective To establish a method for the determination of 1-hydroxy-2-butanone in urine by gas chromatography.Methods Urine samples were acidified with hydrochloric acid,and then stored in the refrigerator.After thawing under natural conditions,urine volume of 2.0 ml was extracted by C18 solid phase,using methanol volume of 2.0 ml elution,detected by gas chromatography with FID detector and quantified by external standard method.Results The measurement range of method is 0.986~32.88 μg/ml,correlation coefficient (r)=0.999 7,detection limit is 0.13 μg/ml;The recovery is 88.1%~92.2%;The precision is 1.4%~ 3.2%.Conclusion This method has a high sensitivity and simple processing.All technical indicators can meet the requirements of the determination method.
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