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LC for 2D‐LC operat...Figure 12.5 Valve systems for column selection (top) and 2D‐LC (bottom).Figure 12.6 Analysis of organohalides in API (promethazine) by SHS‐GC‐MS (SI...Figure 12.7 Analysis of organohalides in API (promethazine) by headspace‐SPM...Figure 12.8 (a) Reaction of sulfonic acid with alcohol and formation of sulf...Figure 12.9 Analysis of sulfonate esters in API (ampicillin) by derivatizati...Figure 12.10 Analysis of sulfonate esters in API (promethazine) by direct in...Figure 12.11 Analysis of N‐mustards in API (doxylamine) by derivatization – ...Figure 12.12 Analysis of Michael reaction acceptors in promethazine spiked a...Figure 12.13 Principle of capillary column back‐flush.Figure 12.14 Analysis of carbamazepine using liquid injection GC‐MS with bac...Figure 12.15 Deans switch 2D‐GC‐MS setup for the analysis of PMI/MI in API b...Figure 12.16 FID monitor detector trace from first dimension separation of t...Figure 12.17 Extracted ion chromatogram from second dimension GC‐MS analysis...Figure 12.18 Analysis of aziridines in Vitamin C spiked at 1 ppm using HILIC...Figure 12.19 RPLC‐MS analysis of non‐derivatized arylamines and aminopyridin...Figure 12.20 RPLC‐MS analysis of derivatized arylamines and aminopyridines i...Figure 12.21 Analysis of 3‐aminobenzonitrile in bupivacaine spiked at 1 ppm ...Figure 12.22 High‐throughput analysis of non‐derivatized arylamine and amino...Figure 12.23 Analysis of hydrazines in Vitamin C spiked at 1 ppm level by de...Figure 12.24 Analysis of phenylhydrazine in Penicillin V spiked at 1 ppm lev...Figure 12.25 Analysis of aldehydes by DNPH derivatization – LC‐MS, Peaks: se...Figure 12.26 TIC and EIC chromatograms for blank solvent (DMSO), spiked solv...Figure 12.27 EIC MRM chromatograms for NDMA, NDMA‐d6, NDEA, NDEA‐d10, NEIPA,...Figure 12.28 EIC chromatograms for NDMA, NDMA‐d6, NMBA, NDEA, NDEA‐d10, NEIP...Figure 12.29 Untargeted analysis of unknown impurities in metoclopramide by ...

      12 Chapter 13Figure 13.1 Diagrammatic representation of how an NMR spectrum is generated....Figure 13.2 The different spin‐states of HB causes the signal from HA to spl...Figure 13.3 The effect of coupling on a single nucleus (a) not coupled and c...Figure 13.4 Quantitative 1H spectra of atenolol (12.36 mg, MW 266.3 g/mol) i...Figure 13.5 The return to equilibrium magnetization is governed by the relax...Figure 13.6 Relative sensitivity of the NMR experiment as a function of magn...Figure 13.7 (a) Traditional and (b) inverse probe designs. The 1H coil is sh...Figure 13.8 A variety of NMR tube diameters: 1, 3, 5, and 10 mm.Figure 13.9 A cryoprobe installation on 600 MHz magnet. The unit on the left...Figure 13.10 The S : N as a function of the number of scans.Figure 13.11 400 mg/ml substrate (a) FID of 19F NMR spectrum with 1H decoupl...Figure 13.12 Relative amplitude as a function of pulse angle for a fixed rel...Figure 13.13 The effect of linewidth on sensitivity. All signals from a sing...Figure 13.14 (a) Simulated spectrum (with no noise) of a substrate signal at...Figure 13.15 1H spectra of H2O (spiked with 5% D2O for a lock) with impuriti...Figure 13.16 Example of the distortion caused by receiver overload. The form...Figure 13.17 2 mM sucrose in 90% H2O. Without water suppression the water si...Figure 13.18 Excitation profiles for rectangular 90° pulses of (a) 10 μs, (b...Figure 13.19 (a) The selective pulse experiment overlaid with (b) a normal c...Figure 13.20 Proton spectra of 100 mg API (4) in d6‐DMSO (a and b) duplicate...Figure 13.21 Proton spectra of 100 mg API (4) in d6‐DMSO (a and b) companion...Figure 13.22 (a) 1H NMR spectrum of TFNB and (b) 50 ppm spike of TFNB in 500...Figure 13.23 19F with 1H decoupling spectra of (a) TFNB and (b) intermediate...Figure 13.24 19F spectrum with 1H decoupling of intermediate (6) at approxim...Figure 13.25 (a) Selective excitation experiment on spiked sample selecting ...Figure 13.26 1H excitation sculpting with double gradient echo exciting the ...Figure 13.27 (a) 1H excitation sculpting with double gradient echo of spikin...Figure 13.28 (a) 1H NMR spectrum of PLGA copolymer highlighting resolved sig...

      13 Chapter 14Figure 14.1 Critical aspects of determining potential degradation products t...Figure 14.2 Proposed process flow for assessing degradation products in the ...Figure 14.3 Illustration of criterion no. 1 in a sample chromatogram: Identi...Figure 14.4 Illustration of combining criterion no. 1 with criterion no. 2 i...Figure 14.5 The degradation pathways of Molecule A in a solid‐oral dosage fo...Figure 14.6 Oxidative stress testing of galunisertib with dilute hydrogen pe...Figure 14.7 Last step in synthesis of galunisertib involves hydrolysis of th...Figure 14.8 PEGylation of MEM‐protected Naloxone.Figure 14.9 Reaction to form AZ13336989 sulphonate ester.Figure 14.10 Degradation pathway of NKTR‐118.Figure 14.11 Degradation pathway of Selumetinib.Figure 14.12 Ames test results for Selumetinib side chain.Figure 14.13 Mechanism of formation of N‐Nitrosamines.Figure 14.14 Potential formation of NDMA inter‐ or intramolecularly within r...Figure 14.15 The proposed drug product workflow for assessing the risk of th...Figure 14.16 Pathway for N‐nitrosation of tertiary amines from nitrites (mor...

      Guide

      1  Cover Page

      2  Title Page

      3  Copyright Page

      4  Preface

      5  Table of Contents

      6  Begin Reading

      7  Index

      8  Wiley End User License Agreement

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