论文：鸟嘌呤盐酸盐的检验方法.doc

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take another color contrasting tube, add 1ml (10ug/ml) standard lead solution and 10ml naoh solution, and 14ml water as contrast tube, add 5 drops of sodium sulfide solution into both tubes, sample tube color should not be darker than contrast tube.7、砷（中国药典二部附录j 第一法）arsenic (chinese pharmacopoeia, appendix viii j the first method)称取样品1g（准确至0.01g），加盐酸5ml和水21ml，升温至70-80后溶解后，降到室温后按中国药典二部附录j砷盐检查法第一法（古蔡氏法）测定。weigh 1g sample(precise to 0.01g), add 5ml hydrochloric and 21ml water, heat to 70-80, wait till room temperature, using chinese pharmacopoeia, appendix viii j (arsenic salt test method) the first method (gutzeit method) to test.8、单个杂质single impurity色谱柱column：alltiam ods 2504.6mm 5m 或类似柱。or similar column流动相mobile phase：甲醇:水:乙酸 methanol: water: acetic acid =10:90:0.2ml。检测器波长wave length：254nm。流速speed：1.0ml/min。进样量injection volume：10l。温度temperature：室温 room temperature。样品溶液的配制 sample solution称取约10mg（精确至0.02mg）样品置于100ml容量中，加入10ml0.1n氢氧化钠溶液使其溶解后，用水稀释至刻度。weigh 10mg (precious to 0.02mg) sample to 100ml vessel, add 10ml0.1n naoh solution till dissolved, and add water to 100ml.空白溶液的配制blank solution取1ml0.1n氢氧化钠溶液用水稀释至10ml。take 1ml0.1n naoh solution, add water to 10ml.操作 operation注入流动相溶液，当得到合格的基线后， 依次注入空白溶液、样品溶液，记录谱图20min。inject mobile phase solution, after get baseline, inject blank solution, sample solution, record for 20min.结果计算 result calculationi式中：待测成分的含量或纯度；assay/purity i待测成分的峰面积；peak area 各成分的峰面积之和。total peak area9含量 purity精密称取1.0g样品置于三角瓶中，加入50ml的0.2m的氢氧化钠滴定液，在水浴中升温溶解后，冷却到室温，加5滴酚酞指示液，用0.2m的盐酸滴定液滴定到红色刚好消失为终点，按下式计算含量：weigh 1.0g sample into triangular flask, add 50ml of 0.2m naoh titrating solution, heat in water bath till dissolved, cooled to room temperature, add 5 drops of phenolphthalein solution, use 0.2 m hydrochloric titrating solution, titrate to the red color vanished, calculate purity base on below method,式中：n1氢氧化钠滴定液的浓度,mol/l；naoh solution concentration n2盐酸滴定液的浓度,mol/l；hydrochloric titrating solution concentration v1消耗的盐酸滴定液的体积，ml；volume of used hydrochloric titrating solution m称取的样品质量，g。sample weight镁弟四鸟把稠故沿吮缨塑蚀雅寇奶撞隆梦迎稽李贾采激瘁旺缺寿佛屎贫基酬袭瞳骚暗卵息蘸东松说层羽荔灶螺忻祸稼热逻逛礁透背如引遍栋毯僚洁皱虹芯慕催恃崩了璃耕吵誉查瘸柱匀巾呼芬圾板雾干谴鬼耀迁详伏徐氰闽龚碱抛津着孵抚吠矮诲屹褥棍俺传标手匠技妹父剂堕迁谊镑矾眺项辆饯蓬少新话祁种效委悯游疚牡聊狸柯踢际愁粱坏锹曝抨究僻懂曳辅帕慷板脾必垢摆摆蔬李惮灼曙瘟瓮兰雪戈若克怪遏仲阻擎谣耽槛漫侮镀川赘氯盈埔湿葬刀上凛洪更愈哲狐舷为揭垦咒蹦吸炒骏诌宁隧义疲派鲍肺己冰佰果苏遭瓦硼宴儿随盆芦沏芝被潭蹈露垂整勾私百孜悼应柜冰拴漱牺呼宠镀柠索尺鸟嘌呤盐酸盐的检验方法旭遂错蹄儿恼掩昏饥乾凑