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Mass Spectrometry: Complex Analysis01:21

Mass Spectrometry: Complex Analysis

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Mass spectrometry is an important technique for the identification of pure compounds. However, it has some limitations for the analysis of complex mixtures, often due to excessive fragmentation making the spectrum too complicated to decipher. Mass spectrometry can be combined with suitable separation methods in sequence, forming hyphenated methods, which are useful in the analysis of complex mixtures.
GC–MS is a powerful hyphenated method commonly used in forensics and environmental...
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¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are...
1.6K
¹H NMR Signal Integration: Overview00:58

¹H NMR Signal Integration: Overview

3.7K
The intensity of a signal, which can be represented by the area under the peak, depends on the number of protons contributing to that signal. The area under each peak is shown as a vertical line called an integral, with the integral value listed under it, as seen in the proton NMR spectrum of benzyl acetate. Each integral value is divided by the smallest integral value to obtain the ratio of the number of protons producing each signal. The ratio reveals the relative number of protons and not...
3.7K
Tandem Mass Spectrometry01:21

Tandem Mass Spectrometry

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Tandem mass spectrometry is a technique that uses multiple mass analyzers in series to obtain a higher selectivity and reduce chemical noise during analyte detection. Instruments with multiple analyzers separated by an interaction cell enable secondary fragmentation and selected study of the fragment ions.Secondary fragmentations occur in the interaction cell and can be induced by various factors. Fragmentation induced by collision with inert gases, such as N2, Ar, He, etc., is called...
2.7K
¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

2.0K
A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied...
2.0K
¹³C NMR: ¹H–¹³C Decoupling01:04

¹³C NMR: ¹H–¹³C Decoupling

1.9K
The probability of having two carbon-13 atoms next to each other is negligible because of the low natural abundance of carbon-13. Consequently, peak splitting due to carbon-carbon spin-spin coupling is not observed in spectra. However, protons up to three sigma bonds away split the carbon signal according to the n+1 rule, resulting in complicated spectra.
A broadband decoupling technique is used to simplify these complex, sometimes overlapping, signals. Broadband decoupling relies on a...
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A Multimodal Wide-Field Fourier-Transform Raman Microscope
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Three New Methods for Resolving Ternary Mixture with Overlapping Spectra: Comparative Study.

Nada Sayed Abdelwahab1, Mona Ali Mohamed2

  • 1Pharmaceutical Analytical Chemistry, Faculty of Pharmacy, Beni-Suef University.

Chemical & Pharmaceutical Bulletin
|June 2, 2017
PubMed
Summary
This summary is machine-generated.

Three new spectrophotometric methods determine metronidazole (MET), diloxanide (DLX), and mebeverine HCl (MEB) simultaneously. These validated methods offer a simple, cost-effective alternative for drug quality control without prior separation.

Keywords:
area under the curvediloxanidemebeverinemetronidazolemodified absorption factormodified amplitude center

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Area of Science:

  • Analytical Chemistry
  • Pharmaceutical Analysis
  • Spectrophotometry

Background:

  • Simultaneous determination of ternary mixtures in pharmaceutical formulations presents analytical challenges.
  • Existing chromatographic methods often require complex separation steps and specialized equipment.
  • Development of rapid, cost-effective analytical techniques is crucial for drug quality control.

Purpose of the Study:

  • To develop and validate novel spectrophotometric methods for the simultaneous determination of metronidazole (MET), diloxanide (DLX), and mebeverine HCl (MEB).
  • To provide alternative analytical methods that avoid prior separation steps.
  • To establish methods suitable for routine drug quality control and laboratories with limited resources.

Main Methods:

  • Development of three spectrophotometric methods: Area Under the Curve (AUC), Modified Absorption Factor (MAFM), and Modified Amplitude Center (MACM).
  • Utilized zero-order and ratio spectra without derivatization.
  • Validated methods using synthetic mixtures and a combined dosage form, assessing linearity, accuracy, and precision per USP guidelines.

Main Results:

  • Successful simultaneous determination of MET, DLX, and MEB was achieved without prior separation.
  • Methods demonstrated good selectivity, accuracy, and precision, with low standard deviation and high percentage recoveries.
  • Statistical comparison using One Way ANOVA confirmed agreement with reported results.

Conclusions:

  • The developed AUC, MAFM, and MACM spectrophotometric methods are reliable and efficient for simultaneous analysis of the ternary mixture.
  • These methods offer a simpler, faster, and more economical alternative to chromatographic techniques for drug quality control.
  • The techniques are easily applicable in quality control settings, especially where advanced instrumentation is unavailable.