Test

USP <Gen. >/

BP [Appndx]

Analytical Method, Target, Analyts

Identification

Identification Tests, General

<191>

Acetate, Aluminum, Ammonium, Antimony, Barium, Benzoate, Bicarbonate, Bismuth, Bisulfite, Borate, Bromide, Calcium, Carbonate, Chlorate, Chloride, Citrate, Cobalt, Copper, Hypophosphite, Iodide, Iron, Lactate, Lead, Lithium, Magnesium, Manganese, Mercury, Nitrate, Nitrite, Oxalate, Permanganate, Peroxide, Phosphate, Potassium, Salicylate, Silver, Sodium, Sulfate, Sulfite, Tartrate, Thiocyanate, Thiosulfate, Zinc

Spectrophotometric Identification Tests

<197>

Infrared Absorption (IR), Ultraviolet Absorption (UV)

Thin-Layer Chromatographic Identification Tests

<201>

TLC

[III A]

Ph. Eur. 2.2.27

Articles of Botanical Origin

<561>

Foreign organic matter, Total ash, Acid-insoluble ash, Water-soluble ash, Alcohol-soluble extractives, Water-soluble extractives, Crude fiber, Starch content, Volatile oil content, Aflatoxins, Pesticide residues (Organophosphorus insecticides, Organochlorine and pyrethroid insecticides)

Identification of articles of botanicals origin

<563>

Diagnostic Plant Morphology and Anatomy, Microtechnique (Microscopic Identification), Chemical Identification (Chemotaxonomy, Active Principles and Marker Compounds

Chromatography

<621>

Paper Chromatography, Thin-Layer Chromatography (TLC), Column Chromatography, Gas Chromatography (GC), High-Pressure Liquid Chromatography (HPLC), Size-Exclusion Chromatography

Lost on Drying

<731>

Volatile matter

Mass Spectrometry

<736>

Gas Chromatography/Mass Spectrometry (GC/MS, GC-MS), Liquid Chromatography/Mass Spectrometry (LC/MS, LC-MS). Ionizations: Electron Impact (EI), Chemical Ionization (CI), Fast Atom Bombardment (FAB). Analyzers: Magnetic Sector, Quadruple, Ion-trap, Time-of-flight (TOF), Fourier Transform. Tandem Mass Spectrometry (MS/MS, MS-MS)

Optical Microscopy

<776>

Microscopic characterization

Spectrophotometry and Light-Scattering

<851>

Ultraviolet, Visible, Infrared, Atomic Absorption, Fluorescence, Turbidimetry, Nephelometry, Roman Measurement

Scan Electron Microscopy

<1181>

Microscopic characterization

Content

Titrimetry

<541>

Titration

Articles of Botanical Origin

<561>

Foreign organic matter, Total ash, Acid-insoluble ash, Water-soluble ash, Alcohol-soluble extractives, Water-soluble extractives, Crude fiber, Starch content, Volatile oil content, Aflatoxins, Pesticide residues (Organophosphorus insecticides, Organochlorine and pyrethroid insecticides)

[XI M]

Tannins in herbal drugs

Chromatography

<621>

Paper Chromatography, Thin-Layer Chromatography (TLC), Column Chromatography, Gas Chromatography (GC), High-Pressure Liquid Chromatography (HPLC), Size-Exclusion Chromatography

Spectrophotometry and Light-Scattering

<851>

Ultraviolet, Visible, Infrared, Atomic Absorption, Fluorescence, Turbidimetry, Nephelometry, Roman Measurement

Safety and Purity

Arsenic

<221>

As

Heavy Metals

<231>

Color comparison method: lead, mercury, bismuth, arsenic, antimony, tin, cadmium, silver, copper, molybdenum

Lead

<251>

Pb

Mercury

<261>

Hg

Residue on Ignition

<281>

Non-volatile impurities, inorganic impurities

Nitrite Titration

<451>

Sulfonamides

Articles of Botanical Origin

<561>

Foreign organic matter, Total ash, Acid-insoluble ash, Water-soluble ash, Alcohol-soluble extractives, Water-soluble extractives, Crude fiber, Starch content, Volatile oil content, Aflatoxins, Pesticide residues (Organophosphorus insecticides, Organochlorine and pyrethroid insecticides)

Botanical Extracts

<565>

Method of Extraction (Percolation, Maceration), Preparations (Fluidextracts, Powdered Extracts, Semisolid Extracts)

Alcohol Determination

<611>

Alcohol

Microbial Enumeration Tests for Nutritional and Dietary Supplements

<2021>

Total Aerobic Microbial Count, Total Combined Molds and Yeasts Count, Enterobacterial Count (Bile-Tolerant Gram-Negative Bacteria)

Microbiological Procedures for Absence of Specific Microorganisms for Nutritional and Dietary Supplements

<2022>

Staphylococcus aureus, Salmonella Species, Escherichia coli (E. coli), Clostridium Species

Microbiological Attributes of Nonsterile Nutritional and Dietary Supplements

<2023>

Microbial contaminations

Impurity

Residue on Ignition

<281>

Non-volatile impurities, inorganic impurities

Ordinary Impurity

<466>

Impurities

Organic Volatile Impurities

<467>

Class 1 Residual Solvents and Their Concentration Limits by USP (ppm): Benzene (2), Carbon tetrachloride (4), 1,2-Dichloroethane (5), 1,1-Dichloroethane (8), 1,1,1-Trichloroethane (1500). Class 2, 3, and Other Residual Solvents. Identification, Control, and Quantification of Residual Solvents

Residue Solvents, Chromatography

<621>

Paper Chromatography, Thin-Layer Chromatography (TLC), Column Chromatography, Gas Chromatography (GC), High-Pressure Liquid Chromatography (HPLC), Size-Exclusion Chromatography

Gel Electrophoresis

<726>

Electrically charged protein, colloids, molecules, or other particles.

Capillary Electrophoresis

<727>

Electrically charged molecules.

Loss on Ignition

<733>

Volatile matters.

Optical Rotation (Specific Rotation)

<781>

Specific rotation: dextrorotatory (+), levorotatory (-), optical isomers, enantiomers, [α]_D²⁵_, [α]_D²⁰

Spectrophotometry and Light-Scattering

<851>

Ultraviolet, Visible, Infrared, Atomic Absorption, Fluorescence, Turbidimetry, Nephelometry, Roman Measurement

Water Determination

<921>

Direct Titration, Residual Titration, Coulometric Titration (Karl Fisher Titration), Azeotropic (Toluene Distillation), Gravimetric.

Physicochemical Characterization

Fats and Fixed Oils

<401>

Specific Gravity, Melting Temperature, Acid Value (Free Fatty Acids), Ester Value, Hydroxyl Value, Iodine Value, Peroxide Value, Saponification Value, Unsaponifiable Matter, Solidification Temperature of Fatty Acids, Fatty Acid Composition, Water and Sediment in Fixed Oils, Anisidine Value, Total Oxidation Value (TOTOX).

[X N]

Identification of fixed oils by TLC, Test for foreign oils by TLC, Test for foreign oils by GC, Sterols in fatty oils

Articles of Botanical Origin

<561>

Foreign organic matter, Total ash, Acid-insoluble ash, Water-soluble ash, Alcohol-soluble extractives, Water-soluble extractives, Crude fiber, Starch content, Volatile oil content, Aflatoxins, Pesticide residues (Organophosphorus insecticides, Organochlorine and pyrethroid insecticides)

Chromatography

<621>

Paper Chromatography, Thin-Layer Chromatography (TLC), Column Chromatography, Gas Chromatography (GC), High-Pressure Liquid Chromatography (HPLC), Size-Exclusion Chromatography

Capillary Electrophoresis (CE)

<727>

Electrically charged molecules.

Mass Spectrometry (MS)

<736>

Gas Chromatography/Mass Spectrometry (GC/MS, GC-MS), Liquid Chromatography/Mass Spectrometry (LC/MS, LC-MS). Ionizations: Electron Impact (EI), Chemical Ionization (CI), Fast Atom Bombardment (FAB). Analyzers: Magnetic Sector, Quadruple, Ion-trap, Time-of-flight (TOF), Fourier Transform. Tandem Mass Spectrometry (MS/MS, MS-MS)

Nuclear Magnetic Resonance (NMR)

<761>

Qualitative or quantitative analysis.

Spectrophotometry and Light-Scattering

<851>

Ultraviolet, Visible, Infrared, Atomic Absorption, Fluorescence, Turbidimetry, Nephelometry, Roman Measurement

Performance Test

Tablet Friability

<1216>

Friability determination of friability of compressed, uncoated tablets.

Dissolution and Disintegration of Dietary Supplements

<2040>

Dissolution, Disintegration

[XII C, D]

Disintegration test for suppositories and pessaries, Dissolution test for transdermal patches

Weight Variation of Dietary Supplements

<2091>

Allowable tablet or capsule weight deviation from the average weight of a sample.

Manufacturing Practices for Dietary Supplements

<2750>

Organizational and Personal: Responsibilities of quality control unit, Personal qualifications, Personal responsibilities. Grounds, Buildings, and Facilities: Grounds, Building designs, Lighting, Ventilation, Air filtration, air heating and cooling, Plumbing, Sewage and refuse, Washing and toilet facilities, General maintenance and sanitation. Equipment: Construction, Cleaning and maintenance, Raw material, product containers and closures, Receipt of storage of untested raw materials, product containers, and closures, Testing and approval or rejection, Use of approved raw materials, product containers and closures, Retesting of approved raw materials, product containers and closures, Reject raw materials, product containers and closures. Production and Process Controls: Written procedures, Charge-in of raw materials, Equipment identification, Sampling and testing in-process materials and dietary products. Labeling and Packaging: Material examination and usage criteria, Labeling issuance, Operations, Temper-resistance packaging, Dietary supplement inspection, Shelf life. Holding and Distribution: Warehousing procedures, Distribution procedures. Quality Control Operations: Testing and release for distribution, Stability testing, Reserve samples. Records and Reports: Master production and control records, Batch production and control records, Laboratory records, Distribution records, Complaint files. Return and Salvaged Products: Returned dietary supplements, Dietary supplement salvaging, Defect action levels