European Directorate for the Quality of Medicines & HealthCare
6
© Council of Europe, 67075 Strasbourg Cedex, France - 2011
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Making copies of this fi le for commercial purpos or posting this fi le on a web site that is open to public consultation is strictly prohibited.
TECHNICAL GUIDE FOR THE ELABORATION OF MONOGRAPHS
6th Edition – 2011血面纱
CONTENTS
1.INTRODUCTION (6)
团队氛围建设
1.1.P URPOSE OF THE G UIDE (6)
1.2.T EST PROCEDURES (6)
1.3.E QUIPMENT (7)
1.4.Q UANTITIES (7)
1.5.R EAGENTS (9)
1.6.C OMMERCIAL NAMES (9)
1.7.R EFERENCE STANDARDS (10)
2.MONOGRAPH ON A SUBSTANCE FOR PHARMACEUTICAL USE (10)
2.1.D EFINITION (11)
2.1.1.Combinations (12)
2.1.2.Content (12)
2.2.C HARACTERS (14)
2.2.1.Appearance (14)
2.2.2.Taste (15)
2.2.3.Odour (15)
2.2.4.Solubility (15)
2.2.5.Stability factors (15)
2.2.6.Hygroscopicity (15)
2.2.7.Solid-state properties (16)
2.2.8.Other characteristics (16)
2.2.9.Behaviour in solution (16)
2.3.I DENTIFICATION (17)
2.3.1.General (17)
2.3.1.1.Methods requiring complex instrumentation (18)
2.3.1.2.Other methods (18)
2.3.2.Infrared absorption spectrophotometry (18)红薯的营养价值
2.3.2.1.Salts of organic acids or bas (18)
2.3.2.2.Chemically related substances (18)
2.3.2.3.Polymorphism (19)
2.3.2.4.Optical isomers (19)
2.3.3.Ultraviolet and visible absorption spectrophotometry (19)
2.3.4.Melting point, freezing point and boiling point (20)
2.3.5.Specific optical rotation (21)
2.3.6.Thin-layer chromatography (21)
2.3.7.Gas chromatography and liquid chromatography (21)
2.3.8.Chemical reactions (22)
2.4.T ESTS (22)
硕士论文答辩
2.4.1.General (22)
2.4.2.Titles (22)
2.4.3.Solution S (23)
2.4.4.Appearance of solution (24)
2.4.4.1.Clarity and degree of opalescence (24)
2.4.4.2.Degree of coloration (25)
2.4.5.pH and Acidity or alkalinity (25)
2.4.6.Optical rotation (27)
保用2.4.7.Absorption spectrophotometry (ultraviolet and visible) (27)
2.4.8.Related substances (28)
2.4.8.1.Thin-layer chromatography (TLC) (32)
2.4.8.2.Liquid chromatography (LC) (33)
2.4.8.3.Gas-liquid chromatography (GC) (37)
2.4.8.4.Capillary electrophoresis (CE) (38)
2.4.9.Readily carbonisable substances (39)
2.4.10.Foreign anions and/or cations (39)
2.4.11.Heavy metals (40)
2.4.12.Loss on drying (41)
2.4.13.Thermogravimetry (2.2.34) (42)
2.4.14.Semi-micro determination of water (Karl Fischer – 2.5.12) (42)
2.4.15.Micro determination of water (2.5.32) (42)
2.4.16.Gas chromatographic determination of water (43)
2.4.17.Determination of water by distillation (2.2.13) (43)
2.4.18.Sulfated ash (2.4.14) (43)
2.4.19.Residue on evaporation (43)
2.4.20.Residual solvents (43)
2.5.A SSAY (44)
2.5.1.Ultraviolet and visible spectrophotometry (44)
2.5.1.1.Direct measurement (44)
2.5.1.2.Measurement after a colour reaction (45)
2.5.2.Volumetric analysis (45)
2.5.3.Chromatography (46)
2.5.4.Determination of nitrogen by sulfuric acid digestion (mi-micro method) (46)
2.6.S TORAGE (46)
2.7.L ABELLING (47)
2.8.I MPURITIES (47)
2.9.F UNCTIONALITY-RELATED CHARACTERISTICS (47)
3.ANALYTICAL VALIDATION (48)
3.1.D EFINITIONS AND TERMINOLOGY (48)
3.1.1.Introduction (48)
3.1.2.Types of analytical procedures to be validated (48)
3.1.3.Validation characteristics and requirements (49)
3.1.4.Glossary (50)
3.2.M ETHODOLOGY (52)
3.2.1.Introduction (52)
3.2.2.Specificity (53)
3.2.2.1.Identification (53)
3.2.2.2.Assays and impurity tests (53)
3.2.3.Linearity (54)
3.2.4.Range (54)
3.2.5.Accuracy (55)
3.2.5.1.Assay (55)
3.2.5.2.Impurities (quantification) (56)
3.2.5.3.Recommended data (56)
3.2.6.Precision (56)
3.2.6.1.Repeatability (56)
3.2.6.2.Intermediate precision (56)
3.2.6.3.Reproducibility (56)
3.2.6.4.Recommended data (57)
3.2.7.Detection limit (57)
3.2.7.1.Bad on visual evaluation (57)
3.2.7.2.Bad on signal-to-noi ratio (57)
3.2.7.3.Bad on the standard deviation of the respon and the slope (57)
3.2.7.4.Recommended data (58)
3.2.8.Quantitation limit (58)
3.2.8.1.Bad on visual evaluation (58)
3.2.8.2.Bad on signal-to-noi ratio (58)
3.2.8.3.Bad on the standard deviation of the respon and the slope (58)
3.2.8.4.Recommended data (59)
3.2.9.Robustness (59)
3.2.10.System suitability testing (59)
3.3.S PECIFIC APPLICATION TO M ETHODS USED IN THE P HARMACOPOEIA (60)
3.3.1.Optical rotation (2.2.7) (60)
3.3.1.1.Introduction (60)
3.3.1.2.Identification (60)
3.3.1.3.Tests (60)
3.3.1.4.Assay (61)
3.3.2.Ultraviolet spectrophotometry (2.2.25) (61)
3.3.2.1.Identification (61)
3.3.2.2.Limit test (61)
衣服起球的原因3.3.2.3.Assay (61)
3.3.3.Non-instrumental limit tests (61)
3.3.3.1.Appearance of solution (2.2.1 and 2.2.2) (61)
3.3.3.2.Acidity or alkalinity (62)
3.3.3.3.Limit tests for anions/cations (2.4) (62)
月嫂工资3.3.4.Atomic absorption spectrometry (2.2.23) (63)
3.3.4.1.Specificity (63)
3.3.4.2.Calibration (63)
3.3.4.3.Matrix effects (64)
3.3.4.4.Detection and quantification limit (bad on the standard deviation of the blank) (64)
3.3.5.Separation techniques (65)
3.3.5.1.Thin-layer chromatography (2.2.27) (65)
3.3.5.2.Liquid chromatography (2.2.29) (66)
3.3.5.3.Gas chromatography (2.2.28) (67)
过国3.3.6.Semi-micro determination of water (2.5.12) (69)
3.3.7.Volumetric titrations (2.5.11; 2.2.19; 2.2.20) (69)
3.3.8.Peptide identification by nuclear magnetic resonance spectrometry (2.2.64) (72)
