[中文]3.1.4.眼科和注射制剂用无添加聚乙烯包装
定义:无添加剂聚乙烯是通过乙烯在高压,有氧条件下或自由基形式的引发剂作为催化剂的条件下聚合获得的。
特性:珠状,颗粒状,粉末状,或通过转化形成不同厚度的透明薄膜或容器。几乎不溶于水,可溶于热的芳香烃,几乎不溶于乙醇,己烷和甲醇,在65℃左右变柔软。
相对密度(2.2.5)为0.910到0.937。
鉴别:如有必要,将待测样品切成最大边长不大于1cm 的碎片。
A. 向0.25g样品中加入10ml甲苯R,在回流冷凝器下煮沸15分钟。向氯化钙中加入几滴上述溶液,放入80℃烘箱中将溶剂蒸发。红外吸收检测(2.2.24)。被测物光谱显示在以下波数处有最大吸收:2920cm-1,2850 cm-1,1465 cm-1,730 cm-1,720 cm-1。得到的光谱与所选标准品的光谱一致。如果待检品是片状,可将其切成适当大小的碎片进行检测。
B. 样品符合添加剂测试(见测试)
测试:如有必要,将待测样品切成最大边长不大于1cm 的碎片。
溶液 S1. 在带有毛玻璃瓶颈的玻璃烧瓶中放入25g样品。加入500ml注射用水R,在回流冷凝器下加热5小时。让其冷却,倾注。取出一部分溶液做外观测试。剩余部分用烧结玻璃滤器过滤(16)。溶液S1在配制后4小时内使用。
溶液 S2.在带有毛玻璃瓶颈的锥形玻璃烧瓶中放入2.0g样品。加入80ml甲苯R,在回流冷凝器下煮沸1.5小时,不断搅拌。允许冷却到60°C并在不断搅拌下加入120ml甲醇R。溶液用烧结玻璃滤器过滤(16)。用40ml甲醇R和60ml甲苯R配成混合溶液,用25ml该混合液冲洗烧瓶和过滤器,将冲洗液加入滤液中,并用同样的混合液稀释到250ml。配制一份空白溶液。
溶液 S3. 在带有毛玻璃瓶颈的锥形玻璃烧瓶中放入100g样品,.加入250ml 0.1M的盐酸,并在回流冷凝器下煮沸1小时,不断搅拌。让其冷却,倾注。
溶液外观. 溶液 S1无色(2.2.2, Method II)澄清(2.2.1)
酸碱度. 向100ml溶液S1中加入0.15m BRP指示剂R。要求0.00M氢氧化钠量不大于1.5ml时指示剂变蓝。向100ml溶液S1中加入0.2ml甲基橙溶液R。要求0.00M甲基橙不大于1.0ml时指示剂开始由黄色变橙色。
吸光度. (2.2.25). 波长在220nm到340nm时,溶液S1吸光度大于0.2。
还原物. 向20ml溶液S1中加入1 ml稀硫酸R和20ml 0.000M高锰酸钾。回流冷凝器下加热3分钟并迅速冷却。加入1g碘化钾R并迅速用0.00M硫代硫酸钠滴定,用0.25ml淀粉溶液R作为指示剂。进行一次空白滴定。消耗滴定液体积差不大于0.5ml。
可溶于己烷的物质. 在250ml带有毛玻璃瓶颈的锥形玻璃烧瓶中放入10g样品。加入100ml己烷R,并在回流冷凝器下煮沸4时,不断搅拌。在冰水中冷却,保持温度在0°C并迅速用烧结玻璃滤器(16)过滤(过滤时间应少于5分钟;如有必要,可以向溶液加压以加快过滤)。
玻璃皿去皮,加入20ml滤液,水浴蒸发。残留物在100-100°C烘箱中干燥1小时。所得残留物的质量在所得标准品残留物的百分之十以内,并且不查过百分之五。
添加剂. 薄层色谱法检测(2.2.27),使用薄层色谱G硅胶板,R。
测试溶液. 在45°C下真空干燥50ml溶液S2至干燥。残渣用5ml二氯甲烷R溶解。根据溶液S2空白溶液配制一份相应的空白溶液。
标准溶液. 在二氯甲烷中溶剂20mg塑料添加剂15CRS和20mg塑料添加剂00CRS,用二氯甲烷稀释到10ml。
在硅胶板上分别加入各溶液10μl。用己烷R展开13cm。让其风干。
展开10cm,用5倍体积甲醇R和95倍体积的二氯甲烷的混合溶液进行二次显影。让其风干,40g/l磷钼酸R的乙醇R溶液喷雾,并在120°C下加热直到标准溶液的色谱中出现斑点。测试溶液色谱中无斑点出现,除了可能在第一次展开时溶剂前沿有一个斑点,且与低聚物一致。忽略所有与空白溶液一致的斑点。得到的标准溶液的色谱上有两个明显的斑点。
可提取重金属 (2.4.8). 将50ml溶液3在水浴中蒸发到大约5ml,并用20ml水R稀释到20ml。取12ml溶液进行检测,符合重金属限度检测A(2.5ppm)。用2.5ml铅标准溶液(10ppm)R配制标准溶液。
炽灼残渣(2.4.14).用5.0g样品进行实验,不大于0.00%
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[外文]3.1.4. POLYETHYLENE WITHOUT ADDITIVES FOR CONTAINERS FOR PARENTERAL PREPARATIONS AND FOR OPHTHALMIC PREPARATIONS
DEFINITION
Polyethylene without additives is obtained by the polymerisation of ethylene under high pressure in the presence of oxygen or free-radical-forming initiators as catalyst.
CHARACTERS
Beads, granules, powder or, after transformation, translucent sheets of varying thickness or containers, practically insoluble in water, soluble in hot aromatic hydrocarbons, practically insoluble in ethanol, in hexane and in methanol. It softens at temperatures above 65 °C. The relative density (2.2.5) of the material is 0.910 to 0.937.
IDENTIFICATION
If necessary, cut the material to be examined into pieces of maximum dimension on a side of not greater than 1 cm.
A. To 0.25 g add 10 ml of toluene R and boil under a reflux condenser for about 15 min. Place a few drops of the solution on a sodium chloride disc and evaporate the solvent in an oven at 80 °C. Examine by infrared absorption spectrophotometry (2.2.24). The spectrum of the substance to be examined shows maxima in particular at some of the following wave-numbers : 2920 cm−1, 2850 cm−1, 1465 cm−1, 730 cm−1, 720 cm−1; the spectrum obtained is identical to that obtained with the material selected for the type sample. If the material to be examined is in the form of sheets, the identification may be performed directly on a cut piece of suitable size.
B. The substance to be examined complies with the test for additives (see Tests).
TESTS
If necessary, cut the material to be examined into pieces of maximum dimension on a side of not greater than 1 cm.
Solution S1. Place 25 g in a borosilicate-glass flask with a ground-glass neck. Add 500 ml of water for injections R and heat under a reflux condenser for 5 h. Allow to cool and decant. Keep part of the solution for the test for appearance of solution. Filter the rest through a sintered glass filter (16). Use solution S1 within 4 h of preparation.
Solution S2. Place 2.0 g in a conical borosilicate-glass flask with a ground-glass neck. Add 80 ml of toluene R and boil under a reflux condenser with constant stirring for 1 h 30 min. Allow to cool to 60 °C and add with continued stirring 120 ml of methanol R. Filter the solution through
a sintered-glass filter (16). Rinse the flask and the filter with 25 ml of a mixture of 40 ml of toluene R and 60 ml of methanol R, add the rinsings to the filtrate and dilute to 250 ml with the same mixture of solvents. Prepare a blanksolution.
Solution S3. Place 100 g in a conical borosilicate-glass flask with a ground-glass neck. Add 250 ml of 0.1 M hydrochloric acid and boil under a reflux condenser with constant stirring for 1 h. Allow to cool and decant the solution.
Appearance of solution. Solution S1 is clear (2.2.1) and colourless (2.2.2, Method II).
Acidity or alkalinity. To 100ml of solution S1 add 0.15ml of BRP indicator solution R. Notmore than 1.5 ml of 0.00 M sodium hydroxide is required to change the colour of the indicator to blue. To 100 ml of solution S1 add 0.2 ml of methyl orange solution R. Not more than 1.0 ml of 0.00 M hydrochloric acid is required to reach the beginning of the colour change of the indicator from yellow to orange.
Absorbance (2.2.25). At wavelengths from 220 nm to 340 nm, the absorbance of solution S1 is not greater than 0.2.
Reducing substances. To 20 ml of solution S1 add 1 ml of dilute sulphuric acid R and 20 ml of 0.000 M potassium permanganate. Boil under a reflux condenser for 3 min and cool immediately. Add l g of potassium iodide R and titrate immediately with 0.00 M sodium thiosulphate, using 0.25 ml of starch solution R as indicator. Carry out a blank titration. The difference between the titration volumes is not more than 0.5 ml.
Substances soluble in hexane. Place 10 g in a 250 ml conical borosilicate-glass flask with a ground-glass neck. Add 100 ml of hexane R and boil under a reflux condenser for 4 h, stirring constantly. Cool in iced water and filter rapidly through a sintered-glass filter (16) maintaining the solution at 0 °C (the filtration time must be less than 5 min; if necessary the filtration may be accelerated by applying pressure to the solution). Evaporate 20 ml of the filtrate in a tared glass dish on a water-bath. Dry the residue in an oven at 100-100 °C for 1 h. The mass of the residue obtained is within 10 per cent of the residue obtained with the type sample and does not exceed 5 per cent.
Additives. Examine by thin-layer chromatography (2.2.27), using a TLC silica gel G plate R.
Test solution. Evaporate 50 ml of solution S2 to dryness in vacuo at 45 °C. Dissolve the evaporation residue with 5 ml of methylene chloride R. Prepare a blank solution from the blank solution corresponding to solution S2. Reference solution. Dissolve 20 mg of plastic additive 15 CRS and 20 mg of plastic additive 00 CRS in methylene chloride R and dilute to 10 ml with the same solvent. Apply to the plate 10 μl of each solution. Develop over a path of 13 cm using hexane R. Allow the plate to dry in air. Carry out a second development over a path of 10 cm
using a mixture of 5 volumes of methanol R and 95 volumes of methylene chloride R. Allow the plate to dry in air, spray with a 40 g/l solution of phosphomolybdic acid R in alcohol R and heat at 120 °C until the spots appear in the chromatogram obtained with the reference solution.
No spot appears in the chromatogram obtained with the test solution, except for a spot which may be at the solvent front from the first development and which corresponds to oligomers. Disregard any spots corresponding to those obtained in the chromatogram with the blank solution. The chromatogram obtained with the reference solution shows
two distinct spots.
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