General Tests, Processes and Apparatus
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GENERAL TESTS, PROCESSES AND APPARATUS General Tests, Processes and Apparatus includes common general test method. methods for tests, useful test methods for quality recognition of drugs and other articles related to them. Unless otherwise 1. Chemical Methods speciˆed, the procedures for acid-neutralizing capacity deter- mination of gastrointestinal medicines, alcohol number de- termination, ammonium determination, arsenic determina- tion, atomic absorption spectrophotometry, test for bacterial 1.01 Alcohol Number endotoxins, boiling point determination, distilling range de- termination, chloride determination, conductivity measure- Determination ment, congealing point determination, determination of bulk Alcohol Number Determination represents the number of and tapped densities, digestion test, disintegration test, disso- milliliters of ethanol at 159C obtained from 10 mL of tin- lution test, endpoint detection in titrimetry, test of extracta- cture or other preparations containing ethanol by the follow- ble volume for injection, ‰ame coloration, ‰uorometry, ing procedures. foreign insoluble matter test for injections, gas chro- matography, heavy metals determination, test for glass Method 1 Distilling method containers for injections, infrared spectrophotometry, This is a method to determine the Alcohol Number by insoluble particulate matter test for injections, insoluble reading the number of milliliters of ethanol distillate at 159C particulate matter test for ophthalmic solutions, iron deter- obtained from 10 mL of a sample measured at 159Cbythe mination, liquid chromatography, loss on drying determina- following procedures. tion, loss on ignition determination, melting point determina- (1) Apparatus tion, test for metal particles in ophthalmic ointments, Use hard glass apparatus as illustrated in Fig. 1.01-1. methanol determination, microbial assay for antibiotics, test Ground glass may be used for the joints. for microbial limit, test for microbial limit for crude drugs, (2) Reagent mineral oil determination, nitrogen determination, nuclear Alkaline phenolphthalein solution: To 1 g of phenolphtha- magnetic resonance spectroscopy, optical rotation determi- lein add 7 mL of sodium hydroxide TS and water to make 100 nation, osmolarity determination, oxygen ‰ask combustion mL. method, particle size distribution test for preparations, pH (3) Procedure determination, test for plastic containers, powder particle Transfer 10 mL of the sample preparation, accurately density determination, powder particle size determination, measured at 15 ± 29C, to the distilling ‰ask A, add 5 mL of test for pyrogen, qualitative test, test for readily carbonizable water and boiling chips. Distil ethanol carefully into the substances, refractive index determination, residual solvents glass-stoppered, volumetric cylinder D. test, residue on ignition determination, test for rubber By reference to Table 1.01-1, a suitable volume of distillate closure for aqueous infusions, speciˆc gravity and density (mL) should be collected, according to the content of ethanol determination, speciˆc surface area determination, test for in the sample preparation. sterility, sulfate determination, thermal analysis, thin-layer Prevent bumping during distillation by rendering the chromatography, test for total organic carbon, ultraviolet- sample strongly acidic with phosphoric acid or sulfuric acid, visible spectrophotometry, uniformity of dosage units (test or by adding a small amount of para‹n, beeswax or silicone for content uniformity, mass variation test), viscosity resin before starting the distillation. determination, vitamin A assay, water determination, and When the samples contain the following substances, carry X-ray powder diŠraction are performed as directed in the out pretreatment as follows before distillation. corresponding articles under the General Tests, Processes (i) Glycerin: Add su‹cient water to the sample so that and Apparatus. The tests for melting point of fats, congeal- the residue in the distilling ‰ask, after distillation, contains at ing point of fatty acids, speciˆc gravity, acid value, saponiˆ- least 50z of water. cation value, ester value, hydroxyl value, unsaponiˆable mat- (ii) Iodine:Decolorizethesamplewithzincpowder. ter and iodine value of fats and fatty oils are performed as (iii) Volatile substances: Preparations containing ap- directed in the corresponding items under Fats and Fatty Oils preciable proportions of essential oil, chloroform, diethyl Test, and sampling, preparation of sample for analysis, ether or camphor require treatment as follows. Mix 10 mL of microscopic examination, purity test, loss on drying, total the sample, accurately measured, with 10 mL of saturated ash, acid-insoluble ash, extract content, and essential oil con- sodium chloride solution in a separator, add 10 mL of tent of crude drugs are performed as directed in the corre- petroleum benzin, and shake. Collect the separated aqueous sponding items under Crude Drugs Test. layer. The petroleum benzin layer was extracted with two 5 Thenumberofeachtestmethodisacategorynumber mL portions of saturated sodium chloride solution. Combine given individually. The number in blackets (<>)appeared the aqueous layers, and distill. According to the ethanol in monograph indicates the number corresponding to the content in the sample, collect a volume of distillate 2 to 3 mL 17 18 Alcohol Number Determination / General Tests JP XV Table 1.01-1 to 2 drops of alkaline phenolphthalein solution, and shake vigorously. If the aqueous layer shows no white turbidity, Ethanol content in Distillate thesample(volz) to be collected (mL) agitate the distillate with additional potassium carbonate. After allowing to stand in water at 15 ± 29C for 30 minutes, more than 80 13 read the volume of the upper reddish ethanol layer in mL, 80 – 70 12 and regard it as the Alcohol Number. If there is no clear 70 – 60 11 boundary surface between these two layers, shake vigorously 60 – 50 10 50 – 40 9 after addition of a few drops of water, then observe in the 40 – 30 8 same manner. less than 30 7 Method 2 Gas chromatography This is a method to determine the alcohol number by deter- mining ethanol (C2H5OH) content (volz) from a sample measured at 159C by the following procedures. (1) Reagent Ethanol for alcohol number: Ethanol (99.5) with deter- mined ethanol (C2H5OH) content. The relation between 15 speciˆc gravity d15 of ethanol and content of ethanol (C2H5OH) is 0.797 : 99.46 volz, 0.796 : 99.66 volz,and 0.795 : 99.86 volz. (2) Preparation of sample solution and standard solution Sample solution: Measure accurately a volume of sample at 15 ± 29C equivalent to about 5 mL of ethanol (C2H5OH), and add water to make exactly 50 mL. Measure accurately 25 mL of this solution, add exactly 10 mL of the internal standard solution, and add water to make 100 mL. Standard solution: Measure accurately 5 mL of ethanol for alcohol number at the same temperature as the sample, and add water to make exactly 50 mL. Measure accurately 25 mL of this solution, add exactly 10 mL of the internal standard solution, and add water to make 100 mL. (3) Procedure Place 25 mL each of the sample solution and the standard solution in a 100-mL, narrow-mouthed, cylindrical glass bottle sealed tightly with a rubber closure and aluminum band, immerse the bottle up to the neck in water, allowed to stand at room temperature for more than 1 hour in a room with little change in temperature, shake gently so as not to splash the solution on the closure, and allow to stand for 30 minutes. Perform the test with 1 mL each of the gas in the bottle with a syringe according to the Gas Chromatography <2.02> under the following conditions, and calculate the ratios, Q T and QS, of the peak height of ethanol to that of the internal standard. Q 5(mL) Alcohol number＝ T × QS a volume (mL) of sample ethanol (C2H5OH) content (volz)of ethanol for alcohol number × 9.406 Internal standard solution—A solution of acetonitrile (3 in 50). Fig. 1.01-1 Operating conditions— Detector: A hydrogen ‰ame-ionization detector. more than that shown in the above Table. Column: A glass tube about 3 mm in inside diameter and (iv) Other substances: Render preparations containing about 1.5 m in length, packed with 150- to 180-mmporous free ammonia slightly acidic with dilute sulfuric acid. If ethylvinylbenzene-divinylbenzene copolymer (mean pore volatile acids are present, render the preparation slightly size: 0.0075 mm, 500 – 600 m2Wg) for gas chromatography. alkaline with sodium hydroxide TS, and if the preparations Column temperature: A constant temperature between contain soap along with volatile substances, decompose the 1059C and 1159C. soap with an excess of dilute sulfuric acid before the extrac- Carrier gas: Nitrogen tion with petroleum benzin in the treatment described in (iii). Flow rate: Adjust the ‰ow rate so that the retention time of To the distillate add 4 to 6 g of potassium carbonate and 1 ethanol is 5 to 10 minutes. JP XV General Tests / Ammonium Limit Test 19 Selection of column: Proceed with 1 mL of the gas ob- tained from the standard solution in the bottle under the above operating conditions, and calculate the resolution. Use a column giving elution of ethanol and the internal standard in this order with the resolution between these peaks being not less than 2.0. 1.02 Ammonium Limit Test Ammonium Limit Test is a limit test for ammonium con- tained in drugs. In each monograph, the permissible limit for ammonium ＋ (as NH4 ) is described in terms