Application of LC-NMR and HR-NMR to the characterization of biphenyl impurities in the synthetic route development for vestipitant, a novel NK1 antagonist

Identification of the Trace Components in BopuzongJian and Macleaya cordata Extract Using LC-MS Combined with a Screening Method

“…However, identifying the impurities from the complex matrix of plant-derived drugs remains a challenge for current analytical techniques. Many instrumental testing methods have been used in previous studies, including gas chromatography-mass spectrometry (GC-MS) [11], liquid chromatographydiode array detection (LC-DAD) [12,13], LC-mass spectrometry (LC-MS) [14,15], capillary electrophoresis-mass spectrometry, and LC-nuclear magnetic resonance (NMR) [15]. LC-MS is playing an increasingly important role in identifying impurities because of its high efficiency of separation, low level of sample consumption, excellent sensitivity, strong specificity, and the ability to provide a wealth of structural information [16,17].…”

Pharmaceuticals and Related Drugs

“…Besides the expanding number of vibrational methods, many UV and NMR methods also have appeared in the literature for carrying out various pharmaceutical measurements. Examples of some of these are summarized in Table . − In one instance, a surface plasmon resonance sensor (PRS) was developed to quantify dextromethorphan in enzyme containing solutions . The PRS is based on an optical fiber bundle with its sensing surface coated with a thin layer of molecularly imprinted β-cyclodextrin polymer.…”

“…Several NMR papers have been published that cover a range of topics including detecting drug counterfeiting using 13 C isotopic measurements, a general procedure for evaluating octanol–water partition coefficients, degradation and purity ,, studies, identity testing of biopharmaceuticals, ,, characterization of crystallinity and polymorphism, , and the complexation of sulfonamides with β-cyclodextrins . In the first example, complete isotopic 13 C profiles were measured for 20 different aspirin and 16 different acetaminophen samples obtained from manufacturers throughout the World.…”

A critical review on the use of modern sophisticated hyphenated tools in the characterization of impurities and degradation products

“…While LC-DQF COSY data identified ␤-glucosidic linkage in the first, LC-2D NMR (HMBC) spectra provided additional key correlation (between 1 H and 13 C) for the second [39]. The combination of LC-NMR and HR-NMR tools was used by Provera et al to characterize an unknown IMP formed in the synthetic route of vestipitant [244], which was not ionized in LC-MS. In this study LC-1 H NMR studies did not provide structural information on the IMP due to complexity in the aromatic region.…”