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Файл:Ординатура / Хирургия / Библиотека им академика М.И. Перельмана / Книга_5491_Библиотеки_им_академика_М_И_Перельмана
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NMR Spectroscopy with Chiral Shift Reagents: NMR spectroscopy can be
enhanced by using chiral shift reagents, which interact differently with
each enantiomer of racemorphan. This technique results in distinct shifts
in NMR peaks, allowing for identification and quantification of individual
enantiomers.
HPLC with Chiral Mobile Phases: In addition to chiral stationary phases,
HPLC can also employ chiral mobile phases. These mobile phases contain
chiral additives that interact differently with each enantiomer, leading to
differential retention times and separation of dextrorphan and
levorphanol.
Capillary Electrophoresis with Chiral Additives: Capillary electrophoresis
can be modified with chiral additives in the electrolyte solution. These
additives selectively interact with the enantiomers of racemorphan,
resulting in differential migration times and separation of the
enantiomers.
Mass Spectrometry with Chiral Reagents: Mass spectrometry can be
coupled with chiral reagents during derivatization to create diastereomers
that exhibit distinct fragmentation patterns. This approach allows for the
identification and quantification of dextrorphan and levorphanol based on
their characteristic mass spectra.
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REMIFENTANIL
IUPAC Name: Methyl 1-(2-methoxycarbonylethyl)-4-(phenyl-propanoyl-amino)-
piperidine-4-carboxylate
Molecular Structure:
Physical Properties:
Appearance: White to off-white crystalline powder
Color: Odorless
Taste: Bitter
Melting Point: 153-157°C
Boiling Point: Decomposes before boiling
Solubility: Slightly soluble in water, freely soluble in methanol and ethanol
Molar Mass: 338.48 g/mol
Chemical Properties:
Chemical Formula: C17H22N3O4
Chemical Classification: Opioid analgesic, Ester
Functional Group: Ester, Amide, Piperidine
pH: Not applicable (solid)
Source or Synthesis: Remifentanil is synthesized in a multi-step chemical process,
typically starting from the amino acid glycine.The exact method is not publicly
known, but it involves multiple chemical reactions and purification procedures.
Route of Administration: Remifentanil is administered intravenously through a
catheter.
Pharmacological Actions: Remifentanil is a potent opioid analgesic that binds to
mu-opioid receptors in the brain and spinal cord. This binding inhibits pain signals
and produces a state of analgesia (pain relief).
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Analysis:
Physical method:
Melting Point (5 °C): Remifentanil has a reported melting point of around
5 °C (41 °F). This involves measuring the temperature at which a solid
sample transitions to a liquid state. While it offers a basic identification
test, the melting point can be influenced by factors like purity and
presence of impurities. It's best used alongside other methods for
confirmation.
X-ray Crystallography: This advanced technique determines the three-
dimensional structure of a molecule by analyzing X-ray diffraction
patterns. By comparing the obtained structure with the known structure
of remifentanil, it can confirm the presence of the drug. However, X-ray
crystallography requires specialized equipment and expertise, limiting its
accessibility.
Chemical method
High-Performance Liquid Chromatography (HPLC): HPLC is widely used
for the quantitative analysis of remifentanil. It separates the components
of a mixture based on their interactions with a stationary phase and a
mobile phase. Remifentanil can be detected and quantified using UV-
visible spectroscopy or mass spectrometry (LC-MS/MS) after separation.
Gas Chromatography (GC): GC is another technique used for the analysis of
volatile compounds. However, since remifentanil is not volatile under
normal conditions, GC might not be the method of choice unless
derivatization is performed to make it volatile.
Mass Spectrometry (MS): MS is often coupled with chromatographic
techniques (like LC-MS/MS or GC-MS) for sensitive and specific detection
and quantification of remifentanil. MS provides information about the
molecular weight and structural information of the compound.
Nuclear Magnetic Resonance (NMR) Spectroscopy: NMR spectroscopy can
be used for structural elucidation and verification of remifentanil. It
provides information about the connectivity of atoms within the molecule.
Spectrophotometric Methods: UV-visible spectrophotometry can be used
for the quantitative determination of remifentanil in solution based on its
absorbance properties at specific wavelengths.
Capillary Electrophoresis (CE): CE can separate charged molecules (like
ionized forms of remifentanil) based on their electrophoretic mobility in
an electric field. It is less commonly used compared to chromatographic
techniques but can be effective.
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SUFENTANIL
Scientific Name: Sufentanil Citrate
IUPAC Name: 2-hydroxypropane-1,2,3-tricarboxylic acid;N-[4-(methoxymethyl)-
1-(2-thiophen-2-ylethyl)piperidin-4-yl]-N-phenylpropanamide.
Molecular Structure:
Physical Properties:
Appearance: White to off-white crystalline powder
Color: Odorless
Taste: Bitter
Melting Point: 222°C (decomposition)
Boiling Point: Not applicable (decomposes before boiling)
Molar Mass: 473.54 g/mol
Solubility:
Water: Slightly soluble (~0.2 grams per 100 mL)
Alcohol: Freely soluble
Chemical Properties:
Chemical Formula: C22H36N2O2S (Sufentanil)
Chemical Classification: Synthetic opioid analgesic, phenylpiperidine
derivative
Functional Groups: Amide, ester, thiophene
Production: Sufentanil is synthesized in a multi-step chemical process from
readily available starting materials. The exact details of the process are proprietary
information owned by the pharmaceutical companies that manufacture it.
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Route of Administration: Sufentanil is typically administered by injection, either
intravenously, epidurally, or intrathecally. It can also be administered sublingually
for the management of breakthrough pain in cancer patients.
Pharmacological Action: Sufentanil binds to and activates opioid receptors in the
brain and spinal cord, producing a powerful analgesic (pain-relieving) effect. It also
causes sedation, respiratory depression, and other side effects.
Analysis:
Physical method
Melting Point Determination:
Principle: Determines the temperature at which sufentanil changes from a
solid to a liquid phase.
Method: A small amount of sufentanil is heated gradually, and the
temperature range over which melting occurs is recorded.
Application: Helps verify the purity and identity of sufentanil by
comparing experimental melting points with known values.
Thermal Analysis:
Techniques: Includes Differential Scanning Calorimetry (DSC) and
Thermogravimetric Analysis (TGA).
Principle: DSC measures heat flow associated with phase transitions
(melting, crystallization), while TGA measures weight change with
temperature (decomposition).
Application: Provides information on thermal behavior, purity, and
stability of sufentanil.
Particle Size Analysis:
Techniques: Such as Laser Diffraction, Dynamic Light Scattering (DLS), or
Microscopy.
Principle: Measures the size distribution of sufentanil particles.
Application: Important for pharmaceutical formulations and ensuring
consistent quality and performance.
Surface Area Analysis:
Techniques: Often involves **BET (Brunauer-Emmett-Teller)** surface
area analysis.
Principle: Measures the specific surface area of sufentanil particles.
Application: Helps understand drug formulation properties and
absorption characteristics.
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Density Measurement:
Principle: Determines the mass per unit volume of sufentanil.
Method: Utilizes techniques like gas pycnometry or liquid displacement
methods.
Application: Assists in calculating dosages and understanding formulation
properties.
Solubility Studies:
Principle: Evaluates how sufentanil dissolves in various solvents or
buffers.
Method: Conducted by observing the dissolution profile or concentration
changes over time.
Application: Important for drug delivery systems and formulation
development.
Powder X-ray Diffraction (XRD):
Principle: Analyzes the crystalline structure of sufentanil.
Method: X-rays are diffracted by the crystal lattice, producing a diffraction
pattern that identifies the crystalline phases.
Application: Confirms the crystalline form and can detect polymorphism
in sufentanil.
Chemical method
High Performance Liquid Chromatography (HPLC):
HPLC is widely used for the quantitative analysis of sufentanil in
pharmaceutical formulations and biological samples. It separates the
components of a mixture based on their interaction with a stationary
phase and a mobile phase.
Detection can be achieved using UV-Vis spectroscopy or mass
spectrometry (MS), which provides sensitivity and specificity in
identifying and quantifying sufentanil.
Gas Chromatography (GC):
GC is another method employed for analyzing sufentanil, especially in
forensic and toxicological contexts.
It involves vaporizing the sample and separating its components based on
their volatility and interaction with the stationary phase inside the
chromatographic column.
Detection is typically done using a suitable detector like a flame ionization
detector (FID) or mass spectrometer.
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Mass Spectrometry (MS):
Mass spectrometry can be used as a standalone technique or coupled with
chromatography (GC-MS or LC-MS) for precise identification and
quantification of sufentanil.
MS ionizes molecules and separates ions based on their mass-to-charge
ratio, providing highly specific and sensitive detection.
Spectroscopic Methods:
Techniques like UV-Vis spectroscopy can be used for qualitative and
quantitative analysis of sufentanil by measuring its absorbance at specific
wavelengths.
Fourier Transform Infrared Spectroscopy (FTIR) can also be used for
structural characterization and qualitative analysis.
Nuclear Magnetic Resonance (NMR):
NMR spectroscopy provides information about the molecular structure of
sufentanil and can be used for qualitative analysis and structural
elucidation.
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THEBACON
Scientific Name: Dihydrocodeinone enol acetate
IUPAC Name:
6, 7-Didehydro-4,5α-epoxy-3-methoxy-17-methylmorphinan-6-ol acetate
Molecular structure
Physical properties:
Appearance: White or colorless crystalline powder
Color: White
Odor: Odorless
Taste: Bitter
Melting point: 212-215°C (414-419°F)
Boiling point: Decomposes before boiling
Molar mass: 341.40 g/mol
Solubility:
Solubility in water: Slightly soluble
Solubility in alcohol: Freely soluble
Chemical properties:
Chemical formula: C20H23NO4
Chemical classification: Opioid, Morphine derivative
Functional groups: Phenolic hydroxyl, acetyl, enol acetate
pH: Not applicable (solid)
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Source: Thebacon is a semisynthetic opioid derived from thebaine, an alkaloid
found in opium poppy.
Route of administration: Oral
Pharmacological action:
Thebacon is an opioid agonist, meaning it binds to opioid receptors in the
brain and spinal cord, producing analgesic (pain-relieving) and antitussive
(cough-suppressing) effects.
It is less potent than morphine but has similar side effects, including
nausea, vomiting, constipation, drowsiness, and dizziness.
Thebacon is no longer commonly used in many countries due to its
potential for abuse and addiction.
Analysis:
Physical method:
Melting Point Determination: The melting point of thebacon can be
determined and compared against known values to confirm its identity
and purity. This method relies on the principle that pure substances melt
at a specific temperature range.
Optical Rotation: Optical rotation can be used to analyze thebacon based
on the rotation of plane-polarized light as it passes through a solution of
the compound. This method can provide information about the
compound's purity and specific optical activity.
Physical Appearance and Solubility: Visual inspection and observation of
the physical appearance of thebacon, such as color, crystal shape, and
solubility in different solvents, can provide initial qualitative information
about the compound.
Microscopy: Microscopic examination of thebacon crystals or powder can
reveal details about its crystal structure, particle size, and morphology,
which can be characteristic and helpful for identification.
X-ray Crystallography: X-ray crystallography is a more advanced physical
method that can be used to determine thebacon's crystal structure at the
atomic level. This technique requires obtaining single crystals of the
compound and analyzing how X-rays are diffracted by the crystal lattice.
Chemical method
High Performance Liquid Chromatography (HPLC):
HPLC is a powerful technique for the quantitative analysis of thebacon in
pharmaceutical formulations and biological samples.
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It separates thebacon from other components in a mixture based on its
interaction with a stationary phase and a mobile phase.
Detection can be achieved using UV-Vis spectroscopy or mass
spectrometry (MS), providing accurate quantification and identification.
Gas Chromatography-Mass Spectrometry (GC-MS):
GC-MS is another effective method for analyzing thebacon, especially in
forensic and toxicological applications.
GC separates thebacon from other compounds based on their volatility,
and MS detects and identifies the separated compounds by their mass-to-
charge ratio.
This method offers high sensitivity and specificity for the identification
and quantification of thebacon.
Nuclear Magnetic Resonance (NMR) Spectroscopy:
NMR spectroscopy can be used for the structural elucidation and
qualitative analysis of thebacon.
It provides information about the chemical structure, connectivity of
atoms, and molecular dynamics of thebacon molecule.
Infrared Spectroscopy (IR):
IR spectroscopy can be utilized for qualitative analysis of thebacon by
identifying functional groups present in the molecule.
It provides information about molecular vibrations and can be used to
confirm the presence of specific bonds characteristic of thebacon.
UV-Vis Spectroscopy:
UV-Vis spectroscopy can be used for the qualitative and quantitative
analysis of thebacon by measuring its absorbance at specific wavelengths.
This method is useful for determining the concentration of thebacon in
solution and can complement other analytical techniques.
Thin-Layer Chromatography (TLC):
TLC can be employed for the qualitative analysis and separation of
thebacon from other substances in a mixture.
It involves separating the components of a mixture based on their affinity
to a stationary phase on a thin layer, followed by visualization under UV
light or by chemical staining.
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