Спецификация на субстанцию «Калия хлорид»
Показатель
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Метод испытания
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Значение нормы
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Описание
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ГФ. Белый кристаллический или гранулированный порошок, или бесцветные кристаллы.
USP.
JP. Potassium Chloride occurs as colorless or white crystals or crystalline powder. It is odorless, and has a saline taste.
EP. White or almost white, crystalline powder or colourless crystals.
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Растворимость
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ГФ. Легко растворим в воде, практически нерастворим в спирте 96 %.
USP.
JP. It is freely soluble in water, and practically insoluble in ethanol (95) and in diethyl ether.
EP. Freely soluble in water, practically insoluble in anhydrous ethanol.
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Подлинность
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ГФ. Кальций. А. К 1 мл раствора соли кальция (2 –20 мг кальций-иона) прибавляют 1 мл аммония оксалата раствора 4 %;
Б. Соль кальция, смоченная хлористоводородной кислотой 25 % и внесенная в бесцветное пламя, окрашивает его в
Хлориды. К 2 мл раствора хлорида (2 – 10 мг хлорид-иона) прибавляют 0,5 мл азотной кислоты, разведенной 16 % и 0,5 мл серебра нитрата раствора 2 %;
USP. Potassium compounds impart a violet color to a nonluminous flame, but the presence of small quantities of sodium masks the color unless the yellow color produced by sodium is screened out by viewing through a blue filter that blocks emission at 589 nm (sodium) but is transparent to emission at 404 nm (potassium).
Chloride. With silver nitrate TS, solutions of chlorides yield a white, curdy precipitate that is insoluble in nitric acid but is soluble in a slight excess of 6 N ammonium hydroxide.
JP. Potassium salt. (1) When the Flame Coloration Test (1) <1.04> is applied to potassium salts, a pale purple color develops.
(2) Neutral solutions of potassium salts yield a white, crystalline precipitate with sodium hydrogen tartrate TS.
(3) Acidic solutions of potassium salts in acetic acid (31) yield a yellow precipitate with sodium hexanitrocobaltate (III) TS.
Chloride. Solutions of chlorides evolve an odor of chlorine, when mixed with sulfuric acid and potassium permanganate, and heated.
Solutions of chlorides yield a white precipitate with silver nitrate TS. When dilute nitric acid is added to a por tion of the separated precipitate, it does not dissolve. When an excess of ammonia TS is added to another portion, the precipitate dissolves.
EP. POTASSIUM
a) Dissolve 0.1 g of the substance to be examined in 2 mL of water R or use 2 mL of the prescribed solution. Add 1 mL of sodium carbonate solution R and heat. No precipitate is formed. Add to the hot solution 0.05 mL of sodium sulfide solution R. No precipitate is formed. Cool in iced water and add 2 mL of a 150 g/L solution of tartaric acid R. Allow to stand. A white crystalline precipitate is formed.
b) Dissolve about 40 mg of the substance to be examined in 1 mL of water R or use 1 mL of the prescribed solution. Add 1 mL of dilute acetic acid R and 1 mL of a freshly prepared 100 g/L solution of sodium cobaltinitrite R. A yellow or orange-yellow precipitate is formed immediately.
a) Dissolve in 2 mL of water R a quantity of the substance to be examined equivalent to about 2 mg of chloride (Cl') or use 2 mL of the prescribed solution. Acidify with dilute nitric acid R and add 0.4 mL of silver nitrate solution Rl. Shake and allow to stand. A curdled, white precipitate is formed. Centrifuge and wash the precipitate with three quantities, each of 1 mL, of water R. Carry out this operation rapidly in subdued light, disregarding the fact that the supernatant solution may not become perfectly clear. Suspend the precipitate in 2 mL of water R and add 1.5 mL of ammonia R. The precipitate dissolves easily with the possible exception of a few large particles which dissolve slowly.
b) Introduce into a test-tube a quantity of the substance to be examined equivalent to about 15 mg of chloride (Cl') or the prescribed quantity. Add 0.2 g of potassium dichromate R and 1 mL of sulfuric acid R. Place a filter-paper strip impregnated with 0.1 mL of diphenylcarbazide solution R over the opening of the test-tube.
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ГФ. Кальций. А. Образуется белый осадок, нерастворимый в уксусной кислоте, разведенной 30 % и аммиака растворе 10 %, растворимый в разведенных минеральных кислотах.
Б. Кирпично-красный цвет.
Хлориды. Образуется белый творожистый осадок, нерастворимый в азотной кислоте, разведенной 16 % и растворимый в аммиака растворе 10 %.
USP. Аналогично ГФ.
JP. Potassium. 1. When it gives a yellow color, a red-purple color can be seen through cobalt glass.
2. The formation of the precipitate is accelerated by rubbing the inside wall of the test tube with a glass rod. The separated precipitate dissolves upon addition of any of ammonia TS, sodium hydroxide TS or sodium carbonate TS.
3. Yellow precipitate.
Chloridum. The gas evolved turns moistened potassium iodide starch paper blue.
A white precipitate.
EP. Potassium. A white crystalline precipitate is formed.
Chloridum. a) A curdled, white precipitate is formed.
b) The paper turns violet-red. The impregnated paper must not come into contact with the potassium dichromate.
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Прозрачность
раствора
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ГФ. 10,0 г субстанции растворяют в 100 мл воды;
USP.
JP. Dissolve 1.0 g of Potassium Chloride in 5 mL of water.
EP.
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ГФ. Полученный раствор должен быть прозрачным.
USP.
JP. The solution is clear and colourless.
EP. Solution S is clear and colourless.
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Цветность
раствора
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ГФ. Раствор, приготовленный в испытании на «Прозрачность раствора», должен быть
USP.
JP. Dissolve 1.0 g of Potassium Chloride in 5 mL of water.
EP.
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ГФ. Бесцветным.
USP.
JP. Colourless.
EP. Сolourless.
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Кислотность и
или щелочность
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ГФ. 10,0 г субстанции растворяют в 100 мл воды. К 50 мл этого раствора прибавляют 0,1 мл 0,05 % раствора бромтимолового синего.
USP. To a solution of 5.0 g in 50 mL of carbon dioxide-free water add 3 drops of phenolphthalein TS.
JP. Dissolve 5.0 g of Potassium Chloride in 50 mL of freshly boiled and cooled water, and add 3 drops of phenolphthalein TS: no red color develops. Then add 0.50 mL of 0.01 mol/L sodium hydroxide VS.
EP. To 50 mL of solution S add 0.1 mL of bromothymol blue solution Rl.
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ГФ. Окраска раствора должна измениться от прибавления не более 0,5 мл 0,01 М раствора натрия гидроксида или не более 0,5 мл 0,01 М раствора хлористоводородной кислоты.
USP. No pink color is produced. Then add 0.30 mL of 0.020 N sodium hydroxide: a pink color is produced.
JP. A red color develops.
EP. Not more than 0.5 mL of 0.01 M hydrochloric acid or 0.01 M sodium hydroxide is required to change the colour of the indicator.
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Щелочноземельные
металлы и магний
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ГФ. К 200 мл воды прибавляют 0,1 г гидроксиламина гидрохлорида, 10 мл буферного раствора аммония хлорида рН 10,0, 1 мл 0,1 М раствора цинка сульфата и 150 мг индикаторной смеси эриохрома черного. Нагревают до температуры 40 °С. Титруют 0,01 М раствором натрия эдетата до перехода окраски из фиолетовой в синюю. К полученному раствору прибавляют 100 мл раствора, содержащего 10,0 г субстанции, и перемешивают. Если цвет раствора изменился на фиолетовый, то его титруют 0,01 М раствором натрия эдетата до появления синего окрашивания. На второе титрование должно пойти не более 5 мл 0,01 М раствора натрия эдетата.
USP. To 20 mL of a solution (1 in 100) add 2 mL each of 6 N ammonium hydroxide, ammonium oxalate TS, and dibasic sodium phosphate TS.
JP. Dissolve 0.20 g of Potassium Chloride in 20 mL of water, add 2 mL of ammonia TS, 2mL of ammonium oxalate TS and 2mL of disodium hydrogenphosphate TS, and then allow to stand for 5 minutes.
EP. To 200 mL of water R add 0.1 g of hydroxylamine hydrochloride R, 10 mL of ammonium chloride buffer solution pH 10.0 R, 1 mL of 0.1 M zinc sulfate and about 15 mg of mordant black 11 triturate R. Heat to about 40 °C. Titrate with 0.01 M sodium edetate until the violet colour changes to full blue. To the solution add the prescribed quantity of the substance to be examined dissolved in 100 mL of water R or use the prescribed solution. If the colour of the solution changes to violet, titrate with 0.01 M sodium edetate until the full blue colour is again obtained.
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ГФ. Не более 0,02 % в пересчете на кальций.
USP. No turbidity is produced within 5 minutes.
JP. No turbidity is produced.
EP. Maximum 200 ppm, calculated as Ca, determined on 10.0 g using 0.15 g of mordant black 11 triturate R. The volume of 0.01 M sodium edetate used does not exceed 5.0 mL.
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Барий
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ГФ. К 5 мл раствора, приготовленного для испытания «Прозрачность раствора», прибавляют 5 мл воды и 2 мл раствора серной кислоты, разведенной 9,8 % и перемешивают.
USP.
JP.
EP. To 5 mL of solution S add 5 mL of distilled water R and 1 mL of dilute sulfuric acid R.
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ГФ. Через 2 ч мутность полученного раствора не должна превышать мутность эталонного раствора, содержащего 5 мл раствора, приготовленного для испытания «Прозрачность раствора», и 7 мл воды.
USP.
JP.
EP. After 15 min, any opalescence in the solution is not more intense than that in a mixture of 5 mL of solution S and 6 mL of distilled water R.
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Железо
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ГФ. К испытуемому и эталонному растворам прибавляют по 2 мл лимонной кислоты раствора 20 % и 0,1 мл тиогликолевой кислоты, перемешивают, добавляют аммиака раствор 10 % до щелочной реакции по универсальной индикаторной бумаге, доводят объем раствора водой до 20 мл, перемешивают и через 5 мин сравнивают окраску растворов.
USP.
JP.
EP. Dilute 5 mL of solution S to 10 mL with water R. Add 2 mL of a 200 g/L solution of citric acid R and 0.1 mL of thioglycollic acid R. Mix, make alkaline with ammonia R and dilute to 20 mL with water R. Prepare a standard in the same manner, using 10 mL of iron standard solution (1 ppm Fe) R.
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ГФ. Не более 0,002 %.
USP.
JP.
EP. Maximum 20 ppm. After 5 min, any pink colour in the test solution is not more intense than that in the standard.
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Мышьяк
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ГФ. К испытуемому и эталонному растворам прибавляют 10 – 12 капель олова(II) хлорида раствора 10 %, 2 г цинка активированного и сразу закрывают колбу пробкой со вставленной в нее верхней частью прибора. Содержимое колбы осторожно взбалтывают и оставляют на 1 ч. При этом температура реакционной смеси не должна превышать 40 °С. Через 1 ч пинцетом извлекают из прибора полоску бумаги и помещают ее в стакан с калия йодида раствором 10 % . Через 10 мин раствор калия йодида сливают, полоску бумаги тщательно промывают несколько раз водой путем декантации в том же стакане и сушат между листами фильтровальной бумаги.
Полоска бумаги, извлеченная из прибора с испытуемым раствором, не должна быть окрашенной или ее окраска не должна быть интенсивнее окраски полоски бумаги, извлеченной из прибора с эталонным раствором.
USP.
JP. Weigh the amount of the sample directed in the monograph, add 5 mL of water, dissolve by heating if necessary, and designate the solution as the test solution.
Place the test solution in the generator bottle A and, if necessary, wash down the solution in the bottle with a small quantity of water. Add 1 drop of methyl orange TS, and after neutralizing with ammonia TS, ammonia solution (28) or dilute hydrochloric acid, add 5 mL of diluted hydrochloric acid (1 in 2) and 5 mL of potassium iodide TS, and allow to stand for 2 to 3 minutes. Add 5 mL of acidic tin (II) chloride TS, and allow to stand for 10 minutes. Then add water to make 40 mL, add 2 g of zinc for arsenic analysis, and immediately connect the rubber stopper H fitted with В and С with the generator bottle A. Transfer 5 mL of the absorbing solution for hydrogen arsenide to the absorber tube D, insert the tip of С to the bottom of the absorber tube D, then immerse the generator bottle A up to the shoulder in water maintained at 25°C, and allow to stand for 1 hour. Disconnect the absorber tube, add pyridine to make 5 mL, if necessary, and observe the color of the absorbing solution: the color produced is not more intense than the standard color.
Preparation of standard color: Measure accurately 2 mL of Standard Arsenic Solution in the generator bottle A. Add 5 mL of diluted hydrochloric acid (1 in 2) and 5 mL of potassium iodide TS, and allow to stand for 2 to 3 minutes. Add 5 mL of acidic tin (II) chloride TS, allow to stand at room temperature for 10 minutes, and then proceed as directed above. The color produced corresponds to 2/jg of arsenic trioxide (AS2O3) and is used as the standard.
EP.
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ГФ. Не более 0,0001 %.
USP.
JP. Not more than 2 ppm.
EP.
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Сульфаты
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ГФ. К 4,5 мл стандартного раствора сульфат-иона спиртового (10 мкг/мл) прибавляют 3 мл бария хлорида раствора 25 %, встряхивают и выдерживают в течение 1 мин.
USP.
JP.
EP. Add 3 mL of a 250 g/L solution of barium chloride R to 4.5 mL of sulfate standard solution (10 ppm SO.,) Rl. Shake and allow to stand for 1 min. To 2.5 mL of this suspension add 15 mL of the prescribed solution and 0.5 mL of acetic acid R. Prepare a standard in the same manner using 15 mL of sulfate standard solution (10 ppm SO.,) R instead of the prescribed solution.
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ГФ. Не более 0,03 %.
USP.
JP.
EP. Maximum 300 ppm. After 5 min, any opalescence in the test solution is not more intense than that in the standard.
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Бромиды
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ГФ. 10,0 г субстанции растворяют в 100 мл воды. 1,0 мл этого раствора помещают в мерную колбу вместимостью 50 мл, доводят объем раствора водой до метки и перемешивают.
К 5,0 мл полученного раствора прибавляют 2,0 мл 1,65 % раствора фенолового красного и 1 мл 0,01 % раствора хлорамина Т и тотчас перемешивают. Точно через 2 мин прибавляют 0,15 мл 0,1 М раствора натрия тиосульфата, перемешивают, доводят объем раствора водой до 10 мл, перемешивают и определяют оптическую плотность раствора на спектрофотометре в максимуме поглощения при длине волны 590 нм, используя воду в качестве раствора сравнения.
USP. Dissolve 2 g of Potassium Chloride in 8 mL of water. Add 1 mL each of chloroform and diluted hydrochloric acid, then add 5 drops of a chloramine T solution (1 in 100), and shake gently.
JP. Dissolve 1.0 g of Potassium Chloride in water to make 100 mL. To 5 mL of the solution add 3 drops of dilute hydrochloric acid and 1 mL of chloroform, and add 3 drops of sodium toluensulfonchloramide TS dropwise while shaking.
EP. Dilute 1.0 mL of solution S to 50 mL with water R. To 5.0 mL of the solution add 2.0 mL of phenol red solution R2 and 1.0 mL of chloramine solution Rl and mix immediately. After exactly 2 min add 0.15 mL of 0.1 M sodium thiosulfate, mix and dilute to 10.0 mL with water R. The absorbance (2.2.25) of the solution measured at 590 nm, using water R as the compensation liquid, is not greater than that of a standard prepared at the same time and in the same manner using 5 mL of a 3.0 mg/L solution of potassium bromide R.
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ГФ. Не более 0,1 %. Оптическая плотность полученного раствора не должна превышать оптическую плотность эталонного раствора, приготовленного таким же образом, но с использованием 5 мл 0,3 % раствора калия бромида вместо испытуемого раствора.
USP. The brown color of the chloroform layer is not darker than that of a concomitantly prepared Standard solution: the limit is 0.1%.
JP. No yellow to yellow-red color develops in the chloroform layer.
EP. Maximum 0.1 per cent.
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Йодиды
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ГФ. 5 г субстанции увлажняют по каплям свежеприготовленной смесью, состоящей из 0,15 мл 10 % раствора натрия нитрита, 2 мл 0,5 М раствора серной кислоты, 25 мл 1 % раствора крахмала и 25 мл воды.
USP. Dissolve 2 g of Potassium Chloride in 8 mL of water. Add 1 mL each of chloroform and diluted hydrochloric acid, then add 2 drops of a chloramine T solution (0.1 in 100), and shake gently.
JP. Dissolve 0.5 g of Potassium Chloride in 10 mL of water, add 3 drops of iron (III) chloride TS and 1 mL of chloroform, shake, allow standing for 30 minutes, and shaking again.
EP. Moisten 5 g by the dropwise addition of a freshly prepared mixture of 0.15 mL of sodium nitrite solution R, 2 mL of 0.5 M sulfuric acid, 25 mL of iodide-free starch solution R and 25 mL of water R. After 5 min, examine in daylight.
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ГФ. Через 5 мин увлажненную субстанцию просматривают при дневном освещении: голубое окрашивание должно отсутствовать.
USP. The violet color of the chloroform layer is not darker than that of a concomitantly prepared Standard solution: the limit is 0.005%.
JP. No red-purple to purple color develops in the chloroform layer.
EP. The substance shows no blue colour.
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Алюминий
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ГФ. Метод 1. Испытуемый раствор помещают в делительную воронку, встряхивают с двумя порциями, по 20 мл каждая, раствора 5 г/л гидроксихинолина в хлороформе, затем с 10 мл этого же раствора. После прибавления каждой порции хлороформные слои отделяют, собирая в мерную колбу вместимостью 50 мл, доводят объем раствора хлороформом до метки и перемешивают. Эталонный и контрольный растворы обрабатывают аналогично.
Измеряют интенсивность флуоресценции испытуемого (I1), эталонного (I2) и контрольного растворов (I3) при длине волны возбуждения 392 нм и длине волны флуоресценции 518 нм. Флуоресценция испытуемого раствора (I1 – I3) не должна превышать флуоресценцию эталонного раствора (I2 – I3).
USP. Determine the absorbances of the Standard Preparations and the Test Preparation at the aluminum emission line at 309.3 nm with a suitable atomic absorption spectrophotometer equipped with an aluminum hollow-cathode lamp and a flameless electrically heated furnace, using the Nitric Acid Diluent as the blank. Plot the absorbances of the Standard Preparations versus the content of Al, in µg per mL, drawing a straight line best fitting the three points. From the graph so obtained, determine the quantity, in µg, of Al in each mL of the Test Preparation. Calculate the amount of Al in the specimen taken, in µg per g, by multiplying this value by 100/W, where W is the weight, in g, of the substance taken to prepare the Test Preparation.
JP.
EP. Place the prescribed solution in a separating fimnel and shake with 2 quantities, each of 20 mL, and then with one 10 mL quantity of a 5 g/L solution of hydroxyquinoline R in chloroform R. Dilute the combined chloroform solutions to 50.0 mL with chloroform R (test solution).
Prepare a standard in the same manner using the prescribed reference solution.
Prepare a blank in the same manner using the prescribed blank solution.
Measure the intensity of the fluorescence (2.2.21) of the test solution (/,), of the standard (/,) and of the blank (I}) using an excitant beam at 392 nm and a secondary filter with a transmission band centred on 518 nm or a monochromator set to transmit at this wavelength.
The fluorescence (/,— I3) of the test solution is not greater than that of the standard (J2- I}).
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ГФ. Не более 0,0001 %.
USP. Proceed as directed using 2.0 g of Potassium Chloride to prepare the Test Preparation: the limit is 1 Mg per g.
JP.
EP. Maximum 1.0 ppm, if intended for use in the manufacture of haemodialysis solutions.
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Натрий
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ГФ. Стандартный и испытуемый растворы разбавляют в соответствии с инструкцией к прибору и проводят определение содержания ионов натрия методом атомной эмиссии (метод прямой калибровки) или атомной абсорбции при длине волны 589 нм.
USP. A solution (1 in 20), tested on a platinum wire, does not impart a pronounced yellow color to a nonluminous flame.
JP. Dissolve 1.0 g of Potassium Chloride in 20 mL of water, and perform the Flame Coloration Test <1.04>.
EP. Atomic emission spectrometry (2.2.22, Method I).
Test solution. Dissolve 1.00 g of the substance to be examined in water R and dilute to 100.0 mL with the same solvent. Reference solutions. Prepare the reference solutions by diluting as required a solution containing 200 |ig of Na per millilitre, prepared as follows: dissolve in water R 0.5084 g of sodium chloride R, previously dried at 105 °C for 3 h, and dilute to 1000.0 mL with the same solvent. Wavelength: 589 nm.
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ГФ. Не более 0,1 %. АЭС или ААС.
USP. No yellow flame.
JP. No persistent, yellow color develops.
EP. Maximum 0.1 per cent, if intended for use in the manufacture of parenteral preparations or haemodialysis solutions.
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Аммоний
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ГФ. К испытуемому и эталонному растворам прибавляют по 0,15 мл реактива Несслера и перемешивают. Через 5 мин сравнивают окраску растворов.
USP.
JP.
EP.
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ГФ. Не более 0,004 %.
USP.
JP.
EP.
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Тяжелые
металлы
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ГФ. Метод 1. К полученным растворам прибавляют по 1 мл уксусной кислоты, разведенной 30 %, 2 капли 2 % раствора натрия сульфида, перемешивают и через 1 мин сравнивают окраску растворов. В сравниваемых растворах допустима слабая опалесценция от выделившейся серы.
Метод 2. К полученным растворам прибавляют по 2 мл ацетатного буферного раствора рН 3,5, перемешивают, прибавляют по 1 мл тиоацетамидного реактива, перемешивают и через 2 мин сравнивают окраску растворов.
USP. Standard Preparation— Into a 50-mL color-comparison tube pipet 2 mL of Standard Lead Solution (20 µg of Pb), and dilute with water to 25 mL. Using a pH meter or short-range pH indicator paper as external indicator, adjust with 1 N acetic acid or 6 N ammonium hydroxide to a pH between 3.0 and 4.0, dilute with water to 40 mL, and mix.
Test Preparation— Into a 50-mL color-comparison tube place 25 mL of the solution prepared for the test as directed in the individual monograph; or, using the designated volume of acid where specified in the individual monograph, dissolve in and dilute with water to 25 mL the quantity, in g, of the substance to be tested, as calculated by the formula: 2.0/(1000L) in which L is the Heavy metals limit, as a percentage. Using a pH meter or short-range pH indicator paper as external indicator, adjust with 1 N acetic acid or 6 N ammonium hydroxide to a pH between 3.0 and 4.0, dilute with water to 40 mL, and mix.
Monitor Preparation— Into a third 50-mL color-comparison tube place 25 mL of a solution prepared as directed for Test Preparation, and add 2.0 mL of Standard Lead Solution. Using a pH meter or short-range pH indicator paper as external indicator, adjust with 1 N acetic acid or 6 N ammonium hydroxide to a pH between 3.0 and 4.0, dilute with water to 40 mL, and mix.
Procedure— Method I - To each of the three tubes containing the Standard Preparation, the Test Preparation, and the Monitor Preparation, add 2 mL of pH 3.5 Acetate Buffer, then add 1.2 mL of thioacetamide–glycerin base TS, dilute with water to 50 mL, mix, allow to stand for 2 minutes, and view downward over a white surface*.
Method II - To each of the tubes containing the Standard Preparation and the Test Preparation, add 2 mL of pH 3.5 Acetate Buffer, then add 1.2 mL of thioacetamide–glycerin base TS, dilute with water to 50 mL, mix, allow to stand for 2 minutes, and view downward over a white surface*.
Method III - Treat the Test Preparation, the Standard Preparation, and the Monitor Preparation as follows. Using a pH meter or short-range pH indicator paper as external indicator, adjust the solution to a pH between 3.0 and 4.0 with ammonium hydroxide (a dilute ammonia solution may be used, if desired, as the specified range is approached), dilute with water to 40 mL, and mix.
To each tube add 2 mL of pH 3.5 Acetate Buffer, then add 1.2 mL of thioacetamide–glycerin base TS, dilute with water to 50 mL, mix, allow to stand for 2 minutes, and view downward over a white surface*.
JP. Place an amount of the sample, directed in the mono graph, in a Nessler tube. Dissolve in water to make 40 mL. Add 2 mL of dilute acetic acid and water to make 50 mL, and designate it as the test solution.
The control solution is prepared by placing the volume of Standard Lead Solution directed in the monograph in a Nessler tube, and adding 2 mL of dilute acetic acid and water to make 50 mL.
EP. Test solution. 12 mL of the prescribed aqueous solution of the substance to be examined.
Reference solution (standard). A mixture of 10 mL of lead standard solution (1 ppm Pb) R or lead standard solution (2 ppm Pb) R, as prescribed, and 2 mL of the prescribed aqueous solution of the substance to be examined.
Blank solution. A mixture of 10 mL of water R and 2 mL of the prescribed aqueous solution of the substance to be examined. To each solution, add 2 mL of buffer solution pH 3.5 R. Mix and add to 1.2 mL of thioacetamide reagent R. Mix immediately. Examine the solutions after 2 min.
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ГФ. Не более 0,001 %.
USP. Dissolve 2.0 g in 25 mL of water: the limit is 0.001%.
M I. The color of the solution from the Test Preparation is not darker than that of the solution from the Standard Preparation, and the color of the solution from the Monitor Preparation is equal to or darker than that of the solution from the Standard Preparation.
M II. The color of the solution from the Test Preparation is not darker than that of the solution from the Standard Preparation.
M III. The color of the Test Preparation is not darker than that of the Standard Preparation, and the color of the Monitor Preparation is equal to or darker than that of the Standard Preparation.
JP. Not more than 5 ppm
EP. Maximum 10 ppm. System suitability: the reference solution shows a slight brown colour compared to the blank solution.
Result: any brown colour in the test solution is not more intense than that in the reference solution.
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Потеря в массе
при высушивании
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ГФ. Если не указано иначе, пробу высушивают в течение 2 ч в сушильном шкафу в пределах температурного интервала, указанного в фармакопейной статье или нормативной документации. Затем открытый бюкс вместе с крышкой помещают в эксикатор для охлаждения на 50 мин, после чего закрывают крышкой и взвешивают. Последующие взвешивания проводят после каждого часа дальнейшего высушивания до достижения постоянной массы. При отсутствии других указаний пробу сушат до постоянной массы при температуре от 100 до 105ºС.
USP. Mix and accurately weigh the substance to be tested, and, unless otherwise directed in the individual monograph, conduct the determination on 1 to 2 g. If the test specimen is in the form of large crystals, reduce the particle size to about 2 mm by quickly crushing. Tare a glass-stoppered, shallow weighing bottle that has been dried for 30 minutes under the same conditions to be employed in the determination. Put the test specimen in the bottle, replace the cover, and accurately weigh the bottle and the contents. By gentle, sidewise shaking, distribute the test specimen as evenly as practicable to a depth of about 5 mm generally, and not more than 10 mm in the case of bulky materials. Place the loaded bottle in the drying chamber, removing the stopper and leaving it also in the chamber. Dry the test specimen at the temperature and for the time specified in the monograph. [note—The temperature specified in the monograph is to be regarded as being within the range of ±2 of the stated figure.] Upon opening the chamber, close the bottle promptly, and allow it to come to room temperature in a desiccator before weighing.
If the substance melts at a lower temperature than that specified for the determination of Loss on drying, maintain the bottle with its contents for 1 to 2 hours at a temperature 5 to 10 below the melting temperature, then dry at the specified temperature.
JP. Weigh accurately a weighing bottle that has been dried for 30 minutes according to the method specified in the mono graph. Take the sample within the range of ± 10% of the amount directed in the monograph, transfer into the weigh ing bottle, and, unless otherwise specified, spread the sample so that the layer is not thicker than 5 mm, then weigh it accu rately. Place the loaded bottle in a drying chamber, and dry under the conditions specified in the monograph. When the size of the sample is large, convert it to small particles having a size not larger than 2 mm in diameter by quick crushing, and use the crushed sample for the test. After drying, remove from the drying chamber, and reweigh accurately. When the sample is dried by heating, the temperature is within the range of ±2°C of that directed in the monograph, and, after drying the bottle, the sample is allowed to cool in a desiccator (silica gel) before weighing.
EP. Determined on 1.000 g by drying in an oven at 105 °C for 3 h.
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ГФ. Не более 1,0 %
USP. Dry it at 105° for 2 hours: it loses not more than 1.0% of its weight.
JP. Not more than 0.5% (1 g, 130°C, 2 hours).
EP. Maximum 1.0 per cent
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Микробиологическая
чистота
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ГФ. В соответствии с требованиями ОФС «Микробиологическая чистота».
USP.
JP.
EP.
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ГФ.
USP.
JP.
EP.
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Бактериальные
эндотоксины
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ГФ. В круглодонные пробирки диаметром 10 мм вносят равные объемы испытуемого раствора и ЛАЛ-реактива (по 0,1 мл). Реакционные смеси аккуратно перемешивают и инкубируют при температуре 37 ± 1 °С в течение 60 ± 2 минут. Во время инкубирования следует избегать вибрации и ударов. По истечении указанного срока визуально регистрируют результаты как положительные или отрицательные. Положительная реакция (+) характеризуется образованием плотного геля, который не разрушается при аккуратном однократном переворачивании пробирки на 180°. Отрицательная реакция (–) характеризуется отсутствием такого геля.
USP.
JP.
EP.
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ГФ. Не более 0,12 ЕЭ на 1 мг калия хлорида.
USP.
JP.
EP.
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Количественное
определение
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ГФ. Около 0,05 г (точная навеска) субстанции растворяют в 50 мл (при потенциометрическом титровании) или 20 мл воды (при определении конечной точки титрования с помощью индикатора) и титруют 0,1 M раствором серебра нитрата потенциометрически или до оранжево-желтого окрашивания (индикатор - 5 % раствор калия хромата). Параллельно проводят контрольный опыт. 1 мл 0,1 М раствора серебра нитрата соответствует 7,455 мг калия хлорида KCl.
USP. Assay— Dissolve about 200 mg of Potassium Chloride, accurately weighed, in 10 mL of water. Add 10 mL of glacial acetic acid, 75 mL of methanol, and 3 drops of eosin Y TS. Titrate, with shaking, with 0.1 N silver nitrate VS to a pink endpoint. Each mL of 0.1 N silver nitrate is equivalent to 7.455 mg of KCl.
JP. Weigh accurately about 0.2 g of Potassium Chloride, previously dried, dissolve in 50 mL of water, and titrate <2.50> with 0.1 mol/L silver nitrate VS while shaking vigorously (indicator: 3 drops of fluorescein sodium TS). Each mL of 0.1 mol/L silver nitrate VS = 7.455 mg of KCl
EP. Dissolve 60.0 mg in water R, add 5 mL of dilute nitric acid R and dilute to 50 mL with water R. Titrate with 0.1 M silver nitrate, determining the end-point potentiometrically (2.2.20). 1 mL of 0.1 M silver nitrate is equivalent to 7.46 mg of KCl.
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ГФ. Содержит не менее 99,0 % (99,5 для парентеральных ЛС) калия хлорида KCl в пересчете на сухое вещество для субстанции
USP. Potassium Chloride contains not less than 99.0 percent and not more than 100.5 percent of KCl, calculated on the dried basis.
JP. Chloride contains not less than 99.0 percent and not more than 100.5 percent of KCl.
EP. Chloride contains not less than 99.0 percent and not more than 100.5 percent of KCl.
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Хранение
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ГФ. В хорошо укупоренной упаковке.
USP. Preserve in well-closed containers.
JP. Tight containers.
EP.
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