第十七改正日本薬局方における国際調和 - Pmda

1 1 1 2 (The European Pharmacopoeia) 3 (The United States Pharmacopeia) 4 5 6 7 8 9 10 11 12 ( ) Rev. Corr. 13 14 15 16 2005 8 (Rev. 2) Residue on Ignition Sulphated Ash Test (Introduction) ( ) Procedure 1.

2 17 2014 6 Thermal analysis (Introduction) ( ) Thermogravimetry 1. Instrument Temperature calibration Calibration of the electrobalance Method Differential scanning calorimetry 2. Instrument Calibration of the instrument Temperature calibration Heat-quantity calibration Operating procedure Applications Phase changes Changes in chemical composition Application to phase diagrams Determination of purity Figure 1 Thermogram 1 Figure 2 Thermal diagrams according to purity 2 Table 1 1 18 19 2 2007 10 Characterisation of Crystalline and Partially

3 Crystalline Solids by X-ray Powder Diffraction (XRPD) X (Introduction) ( ) Principle 1. Instrument 2. Instrument set-up X-ray radiation X Radiation protection Specimen preparation and mounting 3. Specimen preparation Specimen mounting Effect of specimen displacement Effect of specimen thickness and transparency Control of the instrument performance 4. Qualitative phase analysis (Identification of phases) 5. ( ) Quantitative phase analysis 6.

4 Polymorphic samples Methods using a standard Estimate of the amorphous and crystalline fractions 7. Single crystal structure 8. Figure 1 Diffraction of X-rays by a crystal according to Bragg s law 1 X Figure 2 X-ray powder diffraction patterns collected for 5 different solid phases of a substance (the intensities are normalized) 2 X ( ) Figure 3 Geometric arrangement of the Bragg-Brentano parafocusing geometry 3 20 21 22 2013 11 (Rev.)

5 3) Bulk Density and Tapped Density of Powders ( ) Bulk density 1. Method 1 Measurement in a graduated cylinder 1 ( ) Procedure Method 2 Measurement in a volumeter 2 ( ) Apparatus Procedure Method 3 Measurement in a vessel 3 ( ) Apparatus Procedure Tapped density 2. Method 1 1 Apparatus Procedure Method 2 2 Procedure Method 3 3 Procedure Measures of powder compressibility 3.

6 Figure 1 Volumeter 1 Figure 2 Measuring vessel (left) and cap (right) 2 ( ) ( ) Figure 3 3 3 23 2003 11 Specific Surface Area (Introduction) ( ) 1. Multi-point measurement Single-point measurement Sample preparation 2. Outgassing Adsorbate Quantity of sample 3. Method 1 The dynamic flow method 1 Method 2 The volumetric method 2 Reference materials 4. Figure 1 Schematic diagram of the dynamic flow method apparatus 1 Figure 2 Schematic diagram of the volumetric method apparatus 2 24 2007 5 Gas Pycnometric Density of Solids (Introduction) ( ) Apparatus 1.

7 2. Method Expression of the results 3. Figure 1 Schematic diagram of a gas pycnometer 1 ( ) 25 26 4 27 2004 6 ( 1 ) 2007 5 (Rev. 1)( 2 ) ( ) Optical microscopy 1. 1 Apparatus Adjustment Illumination Visual characterization Photographic characterization Preparation of the mount Crystallinity characterization Limit Test of particle size by microscopy Particle size characterization Particle shape characterization General observations Figure 1 Commonly used measurements of particle size 1 Figure 2

8 Commonly used descriptions of particle shape 2 Analytical sieving 2. 2 Principles of analytical sieving Test sieves Test specimen Agitation methods Endpoint determination Sieving methods 1) Mechanical agitation dry sieving method ( ) 2) Air entrainment methods air jet and sonic sifter sieving ( ) Interpretation Figure 1 Commonly used measurements of particle size 1 Figure 2 Commonly used descriptions of particle shape 2 Table 1 Size of standard sieve series in range of interest 1 28 2009 10 29 Water-Solids Interactions - ( ) Introduction Physical states of sorbed water Rates of water uptake Determination of sorption-Desorption Isotherms 1.

9 Principle Methods Report and interpretation of the data Determination of the water activity 2. Principle Methods Figure 1 Example of an apparatus for the determination of the water sorption (other designs are possible) 1 Table 1 Standard saturated salt solutions 1 25 C 30 31 5 2011 6 (Rev. 2) 32 Bacterial Endotoxins Test (Introduction) ( ) Apparatus 1. 2.

10 Preparation of standard endotoxin stock solution Preparation of standard endotoxin solution Preparation of sample solutions Determination of maximum valid dilution 3. Gel-clot technique 4. (1) Preparatory testing (i) Test for confirmation of labeled lysate sensitivity (ii) Test for interfering factors (2) Limit test (i) Procedure (ii) Interpretation (3) Quantitative test (i) Procedure (ii) Calculation and interpretation Photometric quantitative techniques 5.