Proton Nuclear Magnetic Resonance provides detailed insights into the number of hydrogen atoms (protons) and their unique chemical environments within a compound, helping identify its molecular structure with precision
The D₂O Exchange technique in ¹H NMR spectroscopy is a valuable method for identifying exchangeable protons such as –COOH, –OH, –NH, –CONH–, and –SH. When a few drops of D₂O are added to the NMR sample, these protons are replaced by deuterium (forming –COOD, –OD, –ND, –COND, and –SD), causing their signals to disappear from the spectrum, confirming their presence
Carbon-13 Nuclear Magnetic Resonance provides detailed information about the number of carbon atoms present in a compound and their distinct chemical environments, offering valuable insights into the compound’s molecular structure
Fluorine-19 Nuclear Magnetic Resonance reveals the number of fluorine atoms present in a compound and their specific chemical environments, helping to accurately determine the molecular structure and composition
Phosphorus-31 Nuclear Magnetic Resonance provides valuable insights into the number of phosphorus atoms in a compound and their unique chemical environments, aiding in precise structural and compositional analysis
Boron-11 Nuclear Magnetic Resonance offers detailed information about the number of boron atoms in a compound and their surrounding chemical environments, helping to characterize and confirm the molecular structure accurately
WET 1D is a suppression method that selectively removes up to five strong signals, making smaller peaks more visible. When saturating multiple signals, minor artifacts may appear near the suppressed peaks
1D NOESY detects the NOE effect by selectively inverting or saturating a single peak. Its sensitivity is limited due to the use of selective pulses, which restrict magnetization transfer to one proton at a time
The gCOSY experiment helps identify which protons are coupled to each other, providing valuable information about proton–proton connectivity within a molecule
The 13C-HSQC experiment shows one-bond correlations between ¹H and ¹³C atoms. CH and CH₃ groups appear in one color, while CH₂ groups appear in another. It is preferred over HMQC for analyzing crowded carbon spectra
The ¹³C–HMQC experiment also provides one-bond correlations between ¹H and ¹³C. CH and CH₃ appear in one color, and CH₂ in another. HMQC and HSQC offer similar information, differing only in their pulse programs
The ¹³C–HMBC experiment identifies long-range (two- and three-bond) correlations between ¹H and ¹³C atoms. With coupling constants typically ranging from 2 to 14 Hz (default Jₙₓₕ = 8 Hz), it helps distinguish between two-bond and three-bond interactions in complex molecules
The CIGAR experiment detects two-bond and three-bond correlations between ¹H and ¹³C atoms. It allows observation of both ²J and ³J correlation contours without altering the Jₙₓₕ value
The ¹⁵N–HSQC experiment provides one-bond correlations between ¹H and ¹⁵N atoms. In the spectrum, NH and NH₃ groups appear in one color, while NH₂ groups are shown in another
In ROESY spectra, cross-peaks appear opposite in sign to diagonal peaks. This technique is ideal for studying intermediate-sized molecules (kDa range) and smaller molecules in viscous solvents or at low temperatures
2D TOCSY shows correlations between all protons within a spin system, displaying an entire chain of coupled protons for detailed connectivity analysis
VT NMR involves studying nuclei at temperatures above or below ambient to observe their behavior in a magnetic field. High-temperature NMR is particularly useful for confirming rotamers and distinguishing diastereomers and rotamers
qNMR is a powerful technique for assaying compounds without the need for reference standards. It allows accurate quantitative analysis of diverse compound mixtures using NMR signals directly
DOSY measures diffusion coefficients of specific NMR resonances, helping determine the oligomeric state of biomolecules and analyze mixtures of small molecules
The trifluoroacetic acid (TFA) content is determined using ¹⁹F NMR spectroscopy with trifluoromethyl anisole as an external standard
NMR spectroscopy can simultaneously detect and quantify residual solvents with high sensitivity, as these are typically low molecular-weight molecules
Comprehensive NMR analysis, including sequence-specific ¹H NMR assignments, provides conclusive evidence for confirming the chemical structure of compounds, such as peptide antibiotics
Liquid Chromatography-Mass Spectrometry (LC-MS) is an analytical technique that combines the separation power of liquid chromatography with the detection and identification capabilities of mass spectrometry. This method is crucial in the pharmaceutical industry for tasks like drug discovery, development, formulation analysis, and quality control due to its high sensitivity and ability to analyze complex mixtures.
High-Performance Liquid Chromatography, a crucial analytical technique for separating, identifying, and quantifying components in drug mixtures, essential for drug development, quality control (purity, potency), and ensuring product safety and regulatory compliance. It works by forcing a liquid sample under high pressure through a column packed
Gas Chromatography is a important analytical technique for separating, identifying, and quantifying volatile compounds in drug mixtures, essential for quality control, detecting impurities (like residual solvents or genotoxic impurities), ensuring product safety, and meeting regulatory standards like FDA/EMA.
Thermogravimetric Analysis is a technique measuring mass change with temperature to check purity, stability, moisture, decomposition in compounds/products
Differential Scanning Calorimetry is a vital thermal analysis technique used to study drug substances, understand stability, detect impurities, identify crystal forms (polymorphs), and optimize formulations by measuring heat flow changes during temperature transitions like melting or crystallization. It's essential for drug development, ensuring drug efficacy, safety, and consistent quality
Infrared Spectroscopy is a widely used analytical technique in quality control and research. Infrared (IR) spectroscopy helps scientists identify unknown substances, determine the structure of molecules, and detect impurities by measuring how compounds absorb infrared light.
X-ray Diffraction is a crucial non-destructive technique used to analyze the solid-state properties of drug substances, identifying crystal structure, polymorphism (different crystal forms of the same compound, affecting solubility/efficacy), purity, crystallinity, and interactions with excipients, vital for drug development, manufacturing, and quality control.
X-ray fluorescence is a powerful, non-destructive analytical technique used to determine the elemental composition of materials.
Scanning Electron Microscopy is widely used in pharmaceutical research, development, and quality control to study the physical properties, morphology, and chemical composition of various materials.
Transmission Electron Microscopy is a powerful analytical technique used to visualize the internal structure, size, shape, and morphology of materials at a very high resolution, often down to the atomic level.
Inductively Coupled Plasma - Optical Emission Spectroscopy, a powerful analytical technique used to detect and quantify trace metals (elemental impurities) in drug products, raw materials, and biological samples, ensuring purity, safety, and compliance with strict regulations like those from the USP/ICH, crucial for quality control and elemental analysis.
Particle Size Distribution is a measure of the range of particle sizes in a powdered drug (API) or formulation, impacting properties like flow, handling, solubility, and how quickly a drug dissolves (bioavailability).
Heavy metal analysis is the process of detecting toxic metals (like lead, mercury, arsenic, cadmium) in Pharma samples or the environment (water, soil) to assess exposure and poisoning, using techniques like ICP-MS, AAS, or AFS for precise measurement, crucial for health monitoring, industrial safety, and environmental protection.
Potentiometric Titrations are titrating acids/bases or redox reactions without color indicators, finding the equivalence point accurately and also Quantifying the assay of Active Pharmaceutical Ingredients (APIs).
Assay Titrations is a quantitative chemical analysis method to find the exact amount or purity (assay) of a substance (analyte) by reacting it with a solution of known concentration (titrant) until the reaction is complete, signaled by an endpoint (color change/pH shift), using stoichiometry to calculate the analyte's concentration from the titrant volume used.
Residue on Ignition and Loss on Drying are key pharmaceutical tests for purity, but they measure different things: LOD quantifies all volatile matter (water + solvents) lost when a sample is heated (e.g., at 105°C), while ROI measures the inorganic residue left after strong ignition (burning off organic matter at high temp, ~600°C) to find inorganic impurities. Simply put, LOD shows what evaporates, and ROI shows what's left as ash.
Moisture content is the amount of water in a substance, expressed as a percentage or ratio. Melting range is the temperature span over which a substance changes from a solid to a liquid, recorded from the point the first bit of liquid appears to the point where the last bit of solid disappears.
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I highly recommend Accu Analytical Service. They are a reliable and highly expert partner for our analytical needs, demonstrating particular mastery in methods like NMR, HPLC, and GC. We're always impressed by the speed and accuracy with which they deliver their results From Dr.Naveen Kumar Podila Synocule Research Labs Pvt. Ltd
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