为什么用气相色谱法测定制剂中乙醇含量用内标法

2025-03-07 01:38:56
推荐回答(1个)
回答(1):

酒精的作用在医学和法医学上都很有意义。当医生需要知道酒精是否与病人的病情有关时,对血液或尿液中酒精的含量的估计就会起到相当关健的作用。从法医学的观点来看,酒精含量在突然死亡、驾驶事故以及有关以喝醉酒作为防卫性辩解等案件中是至关重要的。决定摄入酒后显示出最大乙醇浓度及量的时间的因素是:对象的体重、乙醇的量及浓度、摄入乙醇的方式、有无食物存在以及对象的身体状况。
酒精的影响对不同的人以及在不同时间的同一个体都是各不相同的。其作用主要取决于各人的所处的环境和体质以及所饮酒精的稀释情况。饮用同等量的酒精对习惯性饮酒者所造成的影响较偶尔饮酒者小得多。药物有加强酒精效果的作用。
很多案例表明,酒精与巴比土酸盐类的协同作用是一些看似是自杀的死亡的一个原因,酒精本身可能是最常见的中毒致死的原因。
装配有火焰离子化检测器及Porapak Q柱的气-固色谱技术在药物制备中一直被用来鉴定和检测乙醇、异丙醇以及丙酮。此项技术是用稀释过的样品的水溶液直接进样, 方法简单而直接。
样品制备 将两份0.5毫升的异丁醇内标物 (浓度为10mg/ml水,其配制法为:用吸量管吸取12.4ml 异丁醇用水稀释至1L ), 用吸量管分别吸入两个不同的2-打兰(7.4毫升)的壳型小瓶中, 一个标为“已知”, 另一个标为“未知”。取0.5ml乙醇作标准物 (浓度为50mg/100ml血液,其配制法为:吸5ml乙醇贮存液,再从血库中取100ml血液加以稀释;所用的乙醇贮存液的配制法为:用水将12.7 ml的无水乙醇稀释至1升),并将其转移至一个标为“已知”的小瓶中。吸量管用内标溶液洗涤三次。用一支10微升的亨氏注射器, 取0.5微升的已知样和未知样各两份进样, 分别测量乙醇和异丁醇的峰高。
 
气相色谱参数 使用一台配有氢火焰检测器的气相色谱仪。火焰离子化检测器可用于检测含水的样品。柱子为不锈钢材料(6英尺×0.25英寸外径), 用30%聚乙二醇2万固定相涂布在用酸洗过的60-80目的Chromosorb W 担体上。柱子用氮气作载气于180°C下吹扫过叶。

操作参数如柱温或载气流速并不是确定不变的,它们可随所研究的化合物的类型及所用气相色谱仪的性质不同而改变。
其它填料也可用于该测定,包括Hallcomid M 180L 涂布在Chromosorb W 80-100 目的担体上或Porapark Q 80-100 目的填料。Porapak 有不同的特性但它的优点是它是一种无需涂层的填料。
注入系统的血液进入进样口并在那里被捕集,而挥发物被载气带入柱中。在柱中进样将会堵塞柱子。所以,如果使用一个长的进样口,将有利于多次进样并能延长使用周期。使用六至八个月后,应将进样口拆开并除去被捕集在此的血液,若有必要,可用水清洗。仪器应在被再次使用前稳定一夜。
根据峰高进行定量测定是令人满意的,但是,若所获得的峰太宽或不对称,也可根据峰面积进行定量。

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