英国药典2012 有关物质项译文

英国药典2012 有关物质项译文
英国药典2012 有关物质项译文

英国药典2012 有关物质项译文

液相色谱法(见2.2.29)

供试品溶液:取20mg本品用2mL乙腈溶解之后,用流动相A稀释至10.0mL。对照溶液(a):去1.0mL待测溶液用流动相A稀释至100.0mL。再取该液1.0mL 用流动相A稀释至10.0mL。

对照溶液(b):取布洛芬杂质B对照品1.0mL用乙腈稀释至10.0mL(溶液A)。取20mg布洛芬标准品用2mL乙腈溶解,加入1.0mL溶液A,并用流动相A稀释至10.0mL。

对照溶液(c):用1mL乙腈溶解布洛芬(峰鉴别用)对照品,并用流动相A稀释至5mL。

色谱柱:

型号:l = 0.15 m, ? = 4.6 mm;

固定相:十八烷基键合硅胶,直径5μm;

流动相:

流动相A:将0.5体积的磷酸和340体积的乙腈、600体积的水混合,平衡后用水稀释至1000体积。

流动相B:乙腈

时间(min)

流动相A

(体积百分比)

流动相B

(体积百分比)

0-25 100 0 25-55 100→15 0→85

相对保留时间:布洛芬保留时间约为21min,杂质J约为0.2min,杂质N约为0.3,杂质A约为0.9,杂质B约为1.1。

系统适应性:对照溶液(b)

峰谷比:最小值1.5;Hp为杂质B的色谱峰顶点至基线的高度,Hv为布洛芬色谱峰和杂质B色谱峰分离的最低点至基线的高度。根据需要调整流动相A中乙腈的浓度。

限度:

杂质A、J、N:每种杂质均不超过对照溶液(a)色谱图中主成分峰面积的1.5倍(0.15%);

非特定杂质:每种杂质均不超过对照溶液(a)色谱图中主成分峰面积的0.5倍(0.05%);

总杂:不超过对照溶液(a)色谱图中主成分峰面积的2倍(0.2%);

忽略限度:对照溶液(a)色谱图中主成分峰面积的0.3倍(0.03%)。

杂质F 气相色谱法(2.2.28)- 使用常规步骤

甲基化溶液:取1mLDMF-DMA和1mL吡啶,用乙酸乙酯稀释至10mL。

供试品溶液:取本品50.0mg于密封小瓶中,用1.0mL乙酸乙酯溶解,加入1mL甲基化溶液,密封,置于烘箱100°C高温加热20min。冷却后,室温氮气吹干,用5mL乙酸乙酯溶解残留物。

对照溶液(a):用乙酸乙酯溶解0.5mg布洛芬杂质F,稀释至10.0mL。

对照溶液(b):取50.0mg布洛芬标准品于密封小瓶中,用1.0mL对照溶液(a)溶解,加入1mL甲基化溶液,密封,置于烘箱100°C高温加热20min。冷却后,室温氮气吹干,用5mL乙酸乙酯溶解残留物。

色谱柱:

填料:石英玻璃

规格:l = 25 m, ? = 0.53 mm

固定相:聚乙二醇20 000(膜厚度2μm)

载气:氦

流速:5.0mL/min

温度:柱温150 °C,注射口200 °C,检测器250 °C

火焰离子化检测

进样量:1μL供试品溶液和1μL对照溶液(b)

运行时间:布洛芬保留时间的两倍

系统适应性:相对保留时间参照布洛芬(保留时间约17min),杂质F≈1.5

限度:杂质F,最高不得超过0.1%

重金属(2.4.8)

最高为10ppm

取12mL溶液S按照试验B方法进行检测。用经甲醇稀释的铅标准溶液(100ppm Pb)制备对照溶液。

药物杂质分析概述

药物杂质分析概述基础导论

药物杂质分析概述基础导论 2

目录 目录 1. 药物杂质分析―概述和法规现状 5 1.1 药物杂质的三个主要类别 6 有机杂质 6 无机(元素)杂质 6 残留溶剂 8 1.2 药品杂质控制的代表性出版物和指南 9 2. 用于药物开发中杂质谱分析的分析技术 11 概述11 2.1 制备型液相色谱 (LC) 12 液相色谱和紫外检测 (LC/UV) 12 液质联用系统 (LC/MS) 13 2.2 气相色谱 (GC) 14 2.3 毛细管电泳 (CE) 14 2.4 电感耦合等离子体发射光谱 (ICP-OES) 和电感耦合 等离子体质谱 (ICP-MS) 15 ICP-OES 15 ICP-MS 15 ICP-MS/MS 16 2.5 超临界流体色谱 (SFC) 16 2.6 傅立叶变换红外光谱仪 (FTIR) 17 3

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