GENERAL TESTS, PROCESSES AND APPARATUS

1 The JP Drugs are to be tested according to the provisions given in the pertinent monographs, GENERAL Notices, GENERAL Rules for Crude Drugs, GENERAL Rules for Preparations, and GENERAL tests for their conformity to the Japanese Pharmacopoeia.(See the GENERAL Notices 5.)25 Table content inthe sample (volz)Distillateto be collected(mL)more than 801380 701270 601160 501050 40940 308less than 30725 GENERAL tests , PROCESSESAND APPARATUSG eneral tests , PROCESSES andApparatus includes commonmethods for tests , useful test methods for quality recognitionof drugs and other articles related to them. Unless otherwisespecified, acid-neutralizing capacity determination of gastro-intestinal medicines, alcoholnumber determination, aminoacid analysis of proteins, ammonium determination, arsenicdetermination, atomic absorption spectrophotometry, boil-ing point determination, chloride determination, conduc-tivity measurement, congealing point determination, deter-mination of bulk and tapped densities, digestion test,disintegration test, dissolutiontest, distilling range determi-nation, endpoint determination in titrimetry, flame colora-tion, fluorometry, foreign insoluble matter test for injec-tions.

2 Foreign insoluble matter test for ophthalmic liquidsand solutions, gas chromatography, glycosylation analysis ofglycoprotein, heavy metal determination, inductively cou-pled plasma-atomic emissionspectrometry and inductivelycoupled plasma-mass spectrometry, infrared spectropho-tometry, insoluble particulate matter test for injections, in-soluble particulate matter test for ophthalmic liquids and so-lutions, iron determination, liquid chromatography, loss ondrying determination, loss onignition determination, massspectrometry, melting point determination, methanol deter-mination, methods for color matching, methods of adhesiontesting, microbial assay for antibiotics, mineral oil determi-nation, nitrogen determination, nuclear magnetic resonancespectroscopy, optical rotationdetermination, osmolarity de-termination, oxygen flask combustion method, particle sizedetermination, particle size distribution test for prepara-tions, pH determination, powder particle density determina-tion, qualitative test, refractive index determination, releasetest for preparations for cutaneous application, residual sol-vents test, residue on ignition determination.

3 Specific gravityand density determination, specific surface area determina-tion, sulfate determination, test for bacterial endotoxins, testfor glass containers for injections, test for metal particles inophthalmic ointments, test for microbial limit, test formicrobial limit for crude drugs,test for plastic containers,test for pyrogen, test for readily carbonizable substances,test for rubber closure for aqueous infusions, test for sterili-ty, test for total organic carbon, test of extractable volumefor injection, thermal analysis, thin-layer chromatography,turbidity measurement, ultravioletvisible spectrophotome-try, uniformity of dosage units (test for content uniformity,mass variation test), viscosity determination, vitamin Aassay, water determination, and X-ray powder diffractionare performed as directed in the corresponding articles underthe GENERAL tests , PROCESSES and APPARATUS .

4 The tests formelting point of fats, congealing point of fatty acids, spe-cific gravity, acid value, saponification value, ester value,hydroxyl value, unsaponifiable matter and iodine value offats and fatty oils are performed as directed in the corre-sponding items under Fats and Fatty Oils Test, and sam-pling, preparation of sample for analysis, microscopic ex-amination, purity test, loss on drying, total ash, acid-insolu-ble ash, extract content, essential oil content of crude drugsand assay of marker compounds for the assay of crude drugsand extracts of Kampo Formulations utilizing nuclear mag-netic resonance (NMR) spectroscopy are performed as di-rected in the corresponding items under the Crude number of each test method is a category numbergiven individually.

5 The number in blackets (<>) appearedin monograph indicates the number corresponding to thegeneral test Chemical Alcohol NumberDeterminationAlcohol Number Determination represents the number ofmilliliters of ethanol at 159C obtained from 10 mL of tin-cture or other preparations containing ethanol by the follow-ing Method 1 Distilling methodThis is a method to determine the Alcohol Number byreading the number of milliliters of ethanol distillate at 159 Cobtained from 10 mL of a sample measured at 159 Cbythefollowing ApparatusUse hard glass APPARATUS as illustrated in Fig. glass may be used for the ReagentAlkaline phenolphthalein solution: To 1 g of phenol-phthalein add 7 mL of sodium hydroxide TS and water tomake 100 ProcedureTransfer 10 mL of the sample preparation, accuratelymeasured at 15 29C, to the distilling flask A, add 5 mL ofwater and boiling chips.

6 Distil ethanol carefully into theglass-stoppered, volumetric cylinder reference to Table , a suitable volume of distil-late (mL) should be collected, according to the content ofethanol in the sample bumping during distillation by rendering the sam-ple strongly acidic with phosphoric acid or sulfuric acid, orby adding a small amount of paraffin, beeswax or siliconeresin before starting the JP Drugs are to be tested according to the provisions given in the pertinent monographs, GENERAL Notices, GENERAL Rules for Crude Drugs, GENERAL Rules for Preparations, and GENERAL tests for their conformity to the Japanese Pharmacopoeia.

7 (See the GENERAL Notices 5.)26 Fig. Alcohol Number Determination/ GENERAL TestsWhen the samples contain the following substances, carryout pretreatment as follows before distillation.(i) Glycerin: Add sufficient water to the sample so thatthe residue in the distilling flask, after distillation, containsat least 50zof water.(ii) Iodine: Decolorize the sample with zinc powder.(iii) Volatile substances: Preparations containing appre-ciable proportions of essential oil, chloroform, diethyl etheror camphor require treatment as follows. Mix 10 mL of thesample, accurately measured, with 10 mL of saturated so-dium chloride solution in a separator, add 10 mL of petro-leum benzin, and shake.

8 Collect the separated aqueous petroleum benzin layer was extracted with two 5 mLportions of saturated sodium chloride solution. Combine theaqueous layers, and distill. According to the ethanol contentin the sample, collect a volume of distillate 2 to 3 mL morethan that shown in the above Table.(iv) Other substances: Render preparations containingfree ammonia slightly acidic with dilute sulfuric acid. Ifvolatile acids are present, render the preparation slightlyalkaline with sodium hydroxide TS, and if the preparationscontain soap along with volatile substances, decompose thesoap with an excess of dilute sulfuric acid before the ex-traction with petroleum benzin in the treatment described in(iii).

9 To the distillate add 4 to 6 g of potassium carbonate and 1to 2 drops of alkaline phenolphthalein solution, and shakevigorously. If the aqueous layer shows no white turbidity,agitate the distillate with additional potassium allowing to stand in water at 15 29C for 30 minutes,read the volume of the upper reddish ethanol layer in mL,and regard it as the Alcohol Number. If there is no clearboundary surface between these two layers, shake vigorouslyafter addition of a few drops of water, then observe in thesame Method 2 Gas chromatographyThis is a method to determine the alcohol number by de-termining ethanol (C2H5OH)content(volz) from a samplemeasured at 159C by the following ReagentEthanol for alcohol number: Ethanol ( ) with deter-mined ethanol (C2H5OH) content.

10 The relation betweenspecific gravityd1515of ethanol and content of ethanol(C2H5OH) is volz, volz, Preparation of sample solution and standard solutionSample solution: Measure accurately a volume of sampleat 15 29C equivalent to about 5 mL of ethanol (C2H5OH),and add water to make exactly 50 mL. Measure accurately25 mL of this solution, add exactly 10 mL of the internalstandard solution, and add water to make 100 solution: Measure accurately 5 mL of ethanolfor alcohol number at the same temperature as the sample,and add water to make exactly 50 mL. Measure accurately25 mL of this solution, add exactly 10 mL of the internalstandard solution, and add water to make 100 ProcedurePlace 25 mL each of the sample solution and the standardsolution in a 100-mL, narrow-mouthed, cylindrical glass bot-tle sealed tightly with a rubber closure and aluminum band,immerse the bottle up to the neck in water, allowed to standat room temperature for more than 1 hour in a room with lit-tle change in temperature, shake gently so as not to splashthe solution on the closure, and allow to stand for 30minutes.