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Pharmacy-Analysis of Barbiturates and Benzodiazepine Sedative-Hypnotic Drugs
This is a mind map about the analysis of pharmaceutical barbiturates and benzodiazepine sedative-hypnotic drugs, including barbiturates, identification tests, related substances and inspections, etc.
Edited at 2023-11-26 20:46:03- cáncer de pulmón
El cáncer de pulmón es un tumor maligno que se origina en la mucosa bronquial o las glándulas de los pulmones. Es uno de los tumores malignos con mayor morbilidad y mortalidad y mayor amenaza para la salud y la vida humana.
- diabetes
La diabetes es una enfermedad crónica con hiperglucemia como signo principal. Es causada principalmente por una disminución en la secreción de insulina causada por una disfunción de las células de los islotes pancreáticos, o porque el cuerpo es insensible a la acción de la insulina (es decir, resistencia a la insulina), o ambas cosas. la glucosa en la sangre es ineficaz para ser utilizada y almacenada.
- sistema digestivo
El sistema digestivo es uno de los nueve sistemas principales del cuerpo humano y es el principal responsable de la ingesta, digestión, absorción y excreción de los alimentos. Consta de dos partes principales: el tracto digestivo y las glándulas digestivas.
Pharmacy-Analysis of Barbiturates and Benzodiazepine Sedative-Hypnotic Drugs
- cáncer de pulmón
El cáncer de pulmón es un tumor maligno que se origina en la mucosa bronquial o las glándulas de los pulmones. Es uno de los tumores malignos con mayor morbilidad y mortalidad y mayor amenaza para la salud y la vida humana.
- diabetes
La diabetes es una enfermedad crónica con hiperglucemia como signo principal. Es causada principalmente por una disminución en la secreción de insulina causada por una disfunción de las células de los islotes pancreáticos, o porque el cuerpo es insensible a la acción de la insulina (es decir, resistencia a la insulina), o ambas cosas. la glucosa en la sangre es ineficaz para ser utilizada y almacenada.
- sistema digestivo
El sistema digestivo es uno de los nueve sistemas principales del cuerpo humano y es el principal responsable de la ingesta, digestión, absorción y excreción de los alimentos. Consta de dos partes principales: el tracto digestivo y las glándulas digestivas.
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- Outline
Analysis of Barbiturates and Benzodiazepine Sedative-Hypnotic Drugs
barbiturates
Structure and properties
Structural features
barbituric acid derivatives
cyclic urea sedative-hypnotics
basic structure
Cyclic malonyl urea structure of parent barbituric acid (common part)
substituent part
Physical and chemical characteristics
Weakly acidic
The mother core cyclic structure contains a 1,3-dimide group Its molecules can undergo keto-enol tautomerism and undergo secondary ionization in aqueous solution.
Slightly acidic Can react with strong bases to form water-soluble salts, usually sodium salts
Barbiturate sodium salt formed by weak acid and strong base, its aqueous solution is alkaline After acidification, crystalline free barbiturates are precipitated, which can be extracted with organic solvents.
Hydrolysis reaction
Contains imide structure It is hydrolyzed by azeotrope with alkali solution, releasing ammonia gas, which can turn red litmus paper blue.
Used to identify amobarbital and barbital
The sodium salt of this type of drug can also undergo hydrolysis under hygroscopic conditions. In general, hydrolysis is slow at room temperature and below pH 10; above pH 11, hydrolysis speeds up as the alkalinity increases.
reaction with metal ions
Contains malonyl urea (-CONHCONHCO-) or imide group
Reacts with silver salts
Contains imide groups
In sodium carbonate solution, sodium salt is formed and dissolved Then with silver nitrate, a soluble silver salt is first generated Adding excess silver nitrate solution will form a white precipitate of insoluble silver salt.
Reacts with copper salts
The enol isomer generated in pyridine solution reacts with copper pyridine test solution Form a stable coordination compound and produce a color reaction similar to biuret
Barbiturates turn purple or form purple precipitates Drugs containing thiobarbiturates appear green
In solutions with higher pH, the purple compounds produced by barbiturates and copper salts with different 5,5-disubstituents have different solubilities in chloroform. The stronger the lipophilicity of the 5,5-disubstituent, the easier it is for the purple compound formed with the copper salt to dissolve in chloroform.
Can be used to differentiate between barbiturates and thiobarbiturates
Preparation of copper pyridine test solution
Dissolve 4g of copper sulfate in 90ml of water, and add 30ml of pyridine to form copper sulfonyl dipyridine complex, that is,
New for temporary use
Reaction with cobalt salts
Reacts with cobalt salt in alkaline solution to form purple coordination compound
The reaction is more sensitive under anhydrous conditions, and the colored products produced are also relatively stable. The reagents used should be free of moisture
Commonly used solvents are anhydrous methanol or ethanol; Cobalt salts are cobalt acetate, cobalt nitrate or cobalt chloride The alkali is preferably an organic base, and isopropylamine is generally used.
reaction with mercury salts
Reacts with mercury nitrate or mercury chloride solution to produce white mercury salt precipitate
This precipitate can be dissolved in ammonia test solution
reaction with vanillin
The hydrogen in its malonyl urea group is relatively active and can undergo a condensation reaction with vanillin in the presence of concentrated sulfuric acid to produce a brown-red product.
BP2009Amobarbital
UV absorption spectral characteristics
The UV absorption spectrum changes significantly with its ionization series.
In acidic solutions, 5,5-disubstituted and 1,5,5-trisubstituted barbiturates do not ionize and have no obvious UV absorption peaks.
In an alkaline solution of pH 10, first-order ionization occurs, forming a conjugated system structure with a maximum absorption peak at a wavelength of 240nm.
In a strong alkaline solution of pH 13, 5,5-disubstituted barbiturates undergo secondary ionization, causing the conjugated system to prolong, causing the absorption peak to red-shift to 255nm.
1,5,5-trisubstituted barbiturates do not undergo secondary ionization due to the presence of the 1-position substituent, and the maximum absorption wavelength is still at 240nm.
The UV absorption spectrum of thiobarbiturates is different
It has obvious UV absorption in acidic or alkaline solutions.
In hydrochloric acid solution (0.1mol/L), the two absorption peaks are at 287nm and 238nm respectively.
In sodium hydroxide solution (0.1mol/L), the two absorption peaks shift to 304nm and 255nm respectively.
In a strong alkaline solution of pH 13, the absorption peak at 255nm disappears and only the absorption peak at 304nm exists.
Thin Layer Chromatography Behavioral Characteristics
Commonly used thin layer chromatography
Microcrystallization
identification test
Chemical identification method
precipitation reaction
Chlorazepam hydrochloric acid solution bismuth potassium iodide → orange-red precipitate
Alprazolam
Alprazolam hydrochloric acid solution bismuth potassium iodide → orange-red precipitate
Alprazolam hydrochloric acid solution Silicotungstic acid solution → white precipitate
Triazolam tablets, chloroform solution, bismuth potassium iodide → orange precipitate
Diazepam injection, flurazepam hydrochloride and its capsules, clonazepam and its injection, Chlorazepam and its tablets, alprazolam and its tablets, triazolam tablets
Sulfuric acid-fluorescence reaction
sulfuric acid
Diazepam – yellow-green
Chlorazepam - yellow
dilute sulfuric acid
Diazepam – Yellow
Chlorazepam – Purple
Estazolam – blue
Estazolam and its tablets and injections, diazepam and its tablets
Chloride identification reaction
Chloride reaction after destruction by oxygen bottle combustion method
Diazepam, midazolam, flurazepam hydrochloride and their capsules
Reactions of primary aromatic amines
1-N is unsubstituted. It can be thermally hydrolyzed with hydrochloric acid to form aromatic primary amines. Identification by diazotization-coupling reaction
Color developer: Naphthylethylenediamine hydrochloride
Chlorazepam - red-purple
Spectroscopy
UV spectrophotometry
UV maximum absorption wavelength Absorbance or absorbance ratio at the maximum absorption wavelength
typical drugs
Infrared absorption spectrum
API - Infrared Spectrophotometry
Preparations—Post-extraction infrared spectrophotometry
NMR
Obtain direct information about drug molecule skeleton, configuration and conformation
Basis: chemical shift, coupling constant and resonance peak integrated intensity
chromatography
thin layer chromatography
ChP Nitrazepam Tablets
BP Clonazepam and Chlorazepam
USP Diazepam and Flurazepam Hydrochloride
HPLC
ChP Lorazepam API and its preparations, midazolam and its injection, , Clonazepam Tablets and Diazepam Injection Clonazepam
Related substances and inspections
Typical impurities
Has a "benzophenone" structure
Validity check
triazolam
ChP small cup method for dissolution determination
USP Chromatographic Determination Using Paddle Method for Large Volume Injection
Content determination
volumetric titration
Non-aqueous alkali method
Perchloric acid nonaqueous solution titration of typical drugs
non-aqueous acid method
Titrant: Tetrabutylammonium hydroxide
Oxazepam, Lorazepam