N-oxide metabolites have the same elemental composition as those metabolites resulting from hydroxylation. We use cookies to help provide and enhance our service and tailor content and ads. Through first reacting the sample to bring the metal into solution as an ion, the trace metal content of an alloy, such as manganese in steel, can be determined. This article explores the above recent applications of Raman spectroscopy in the pharmaceutical field. Spectrophotometric methods play an important role in the generation of this data, and the evaluation of the risks associated with this process, thereby assisting compliance. How? This can be performed by stepwise hydrolysis accompanied with chromatography. In this, triple quadrupole mass spectrometer along with LSI-MS was employed [23]. Therefore, base molecular formula will be: Hydrogen atoms in predicted base molecular formula = 14. Pharmaceutical spectroscopy equipment comes in many forms, and its variety makes it accessible to a broad range of research professionals working within diverse budgets. A variety of analyte separation techniques like capillary electrophoresis, gas chromatography and high-performance liquid chromatography are united with mass spectroscopy for simultaneous separation and determination of analytes called CE-MS, GC–MS and HPLC-MS, respectively. 1. Stable isotope-labeled (2H, 13C, 15N, 18O, 34S and others) xenobiotics can facilitate metabolite detection and identification by mass spectrometry, especially when radiolabeled parent drug is not available [46–48]. Copyright © 2014 Elsevier Inc. All rights reserved. This library consisted of 17 commonly encountered drugs in parenteral pharmaceutical formulations, that is, surgical analgesic: fentanyl, hydromorphone and morphine; anesthetic: baclofen, bupivacaine, ketamine, midazolam, ropivacaine and succinylcholine; and a mixture of other drug classes: caffeine, clonidine, dexamethasone, ephedrine, heparin, methadone, oxytocin and phenylephrine [37]. Under normal healthy condition, only small quantities of bile acids are found in peripheral circulation and urine, but in hepatobiliary and intestinal diseases it will get affected. Peptides are converted into amino alcohols which are volatile in nature. The characterization of commercial prebiotic galacto-oligosaccharide mixture was done with linear ion-trap mass spectrometer coupled with high-performance anion-exchange chromatography (HPAEC) using electrospray ionization combination with 1H NMR and 13C NMR [15]. It is based on the conversion of the sample into ionized state, with or without fragmentation which are then identified by their mass-to-charge ratios (m/e). APPLICATIONS OF UV SPECTROPHOTOMETRY IN PHARMACEUTICALS • Qualitative analysis through spectrophotometric methods achieves fast and accurate results using only small sample quantities. Applications Spectroscopy is used as a tool for studying the structures of atoms and molecules. Therefore, it is considered as trace analysis methodology. Abstract This chapter covers the use of spectrophotometry in the pharmaceutical industry. Two drugs lopinavir and ritonavir were analyzed and described that HIV protease inhibitors can successfully be quantified in peripheral blood mononuclear cells using MALDI-TOF mass spectrometry [36]. Both of these transformations involve changes in the molecular weight. Application of Mass Spectroscopy in Pharmaceutical and Biomedical Analysis, Spectroscopic Analyses - Developments and Applications, Eram Sharmin and Fahmina Zafar, IntechOpen, DOI: 10.5772/intechopen.70655. Fragment ion peak: Peak of fragment ion in mass spectrum is called fragment ion peak. 6-OH desloratadine and N-oxides can be clearly differentiated as the major fragment ion from N-oxides was due to the loss of an oxygen atom while the prominent fragment ion from 6-OH desloratadine was due to loss of H2O [45]. Despite the need for improvement, mass spectrometry will become popular in the near future with fast turnaround times, ease of use and potential operational cost savings [32]. However, cases of murders or death due to poisoning and drug overdose are also the prime targets for these drug candidates’ analysis [38]. It is generated due to loss of kinetic energy of ion during acceleration from ionization chamber to analyzer tube. history and applications of near infrared spectroscopy The discovery of the infrared region in 1800 is credited to William F. Hershel's famous work, "Experiments on the Refrangibility of the Invisible Rays of the Sun", read April 24, 1800 at the Royal Society, Phil. APPLICATIONS OF FLAME EMISSION SPECTROSCOPY IN PHARMACEUTICAL ANALYSIS . The sample for forensics in the case of drug abuse is mainly urine, hair and blood. Raman spectroscopy provides a molecular level insight into processing, and therefore it is a future process analytical tool. As PhD students, we found it difficult to access the research we needed, so we decided to create a new Open Access publisher that levels the playing field for scientists across the world. The presence of an analyte gives a response which can be assumed to be proportional to the concentration. Important deficiencies in present MALDI-TOF MS platforms include misclassification such as of Shigella as Escherichia coli and Streptococcus pneumoniae as Streptococcus mitis and, additionally, poor performance with polymicrobial samples. These range from water and waste water analysis, pharmaceutical quality control and food analysis, such as the grading of olive oil to meet European regulations ECC/2568/91 and 2472/97. Spectroscopy is the measurement and interpretation of electromagnetic radiation absorbed or emitted when the molecules or atoms or ions of a sample moves from one energy state to another energy state. This technique, not only elucidates the structure of the compounds, but also provides the information of molecular formula and the isotopic abundance of particular molecular formula. It is divided into two parts: If m/e value of molecular ion peak is odd number, then it may contain odd number of nitrogen atoms. It can be represented by m + 1 and m + 2 for one and two molecular weight higher isotopes and vice versa for lower weight isotopes. Similarly, RNA polymerase II (Pol II) transcription initiation complex structure was analyzed by cross-linking and mass spectroscopy. We are a community of more than 103,000 authors and editors from 3,291 institutions spanning 160 countries, including Nobel Prize winners and some of the world’s most-cited researchers. The large number of wavelengths emitted by these systems makes it possible to investigate their structures in detail, including the electron configurations of ground and various excited states. Mass spectrum is produced in the form of bar graph which is interpreted by using the following peaks. Absorption spectroscopy is an important analytical chemistry technique used in pharmaceutical analysis. Mass spectroscopy provides rich elemental information, which is an important asset to interpret complex mixture components. Hydrogen atoms in actual molecular formula of compound = 4. Moreover, steady-state, near-infrared spectroscopy is a very significant tool in pharmaceutical analysis. Steps for determination of hydrogen deficiency index: Make the correction in the predicted base formula with respect to the elements obtained from other spectral data, and the correction requires addition or removal of hydrogen atoms, which depends upon the type of element added. Detection of Impurities UV absorption spectroscopy is one of the best methods for determination of impurities in organic molecules. Login to your personal dashboard for more detailed statistics on your publications. The variations and permutation combinations of different ionization techniques with the different analyzers provide the analysis of diversified chemical entities at the femtogram level. Analytes having high molecular weight and temperature sensitive can be efficiently analyzed by HPLC coupled with atmospheric pressure ionization-mass spectrometer (API-MS) [1]. Avantes specializes in the development of high-resolution, high-sensitivity spectrometers and is a reliable option for hundreds of researchers and original equipment manufacturers in biomedical applications. The state-of-the-art and possibilities offered by derivative spectrophotometry in the field of pharmaceutical analysis during the period 2008 – 2012 are reviewed. Mass spectroscopy emerged as a powerful tool for various operations in pharmaceutical field mainly in drug development. By Tünde Jurca, Eleonora Marian, Laura Graţiela Vicaş, Mariana Eugenia Mureşan and Luminiţa Fritea. Mass spectroscopy has major use in structure elucidation of compounds. Mass spectrometry (MS) is an advanced technique for determining the molecular weight of a compound. The spectrophotometer technique is to measure light intensity as a function of wavelength. 5. Mass spectroscopy is the favored method for endocrine disorders analysis, for example, steroid analysis which requires technical competence, skill and experience for the needed improvement [24]. It shows promising results in its ability to visualize the drug and excipients distribution in pharmaceutical formulations such as tablets, creams and ointments. Therefore, base molecular formula will be: Hydrogen atoms in predicted base molecular formula = 6. Last Updated on January 4, 2020 by Sagar Aryal. This occurs due to disturbances in synthesis and pharmacokinetics in the body. This approach was applied to differentiate sulfoxide and sulfone metabolites from the isomeric mono- and di-hydroxylated metabolites, respectively. The peptide sequence was analyzed using combination of gas-phase ion/ion chemistry and tandem mass spectrometry. The mass spectroscopy is based on the positive ion generation. Hydrogen deficiency index is 4, because four pairs of hydrogen atoms are required to saturate the compound. Matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) emerged as a valuable tool in direct analysis of pharmaceutical formulations. Copyright © 2021 Elsevier B.V. or its licensors or contributors. These are often used as characteristic of a compound for identification. Some of the drugs in routine analysis include opiates, cocaine, marihuana, lysergic acid diethylamide (LSD) and amphetamines. Analysis of methadone and its metabolites with other illicit drugs like cocaine, phencyclidine, heroin and 6-acetylmorphine in hair by GC–MS is another successful application of mass spectroscopy [43]. Hydrogen deficiency index(HDI): Number of pairs of hydrogen required to saturate the compound is called hydrogen deficiency index (HDI). By continuing you agree to the use of cookies. This fast and effect instrumentation has become an essential tool in the pharmaceutical industry thanks to its adaptability and economic value. Built by scientists, for scientists. Fragmentation pattern is characteristic for a particular organic compound. The applications where these spectroscopic techniques are used provide a significant contribution to the analytical process. They used peptide drugs as an example and used ion trap mass spectrometer with electrospray ionization in their method [34]. Recent research has looked into the possible applications of mass spectrometers in biomedical field. Licensee IntechOpen. Similarly, benzene ring has hydrogen deficiency index four because it contains three double bonds and one ring in it. Mass spectroscopy now becomes an irreplaceable tool in all types of drug discoveries due to its high sensitivity, speed, versatility and selectivity [33]. The ease of use, ability to run large numbers of isolates per batch, simplicity of setup, automation, rapid turnaround time and low reagent costs are the major advantages. To date our community has made over 100 million downloads. Indeed, it is suitable for analysis of solid, liquid, and biotechnological pharmaceutical forms. In forensic study, sample is in minute quantity; therefore, high sensitivity is required for analysis. Implementation of mass spectroscopy in clinical laboratory resulted in significant advancements. In some cases, instruments have identified only one organism without indicating the presence of others. Matrix-assisted laser desorption/ionization imaging mass spectrometry is emerged as a potent instrument for the investigation of small molecules and proteins in biological systems by in situ analysis of tissue sections [28]. They employed linear ion trap quadrupole (LTQ)-orbitrap spectrometer and recorded Fourier transform mass spectrometer (FTMS) spectra at 100,000 resolutions. Ionization of molecule by electron bombardment. It is also a noninvasive tool that permits in vivo studies in humans. The development of double and triple quad techniques and their application have definitely uplifted the level of research and analysis in biomedical field, and this chapter gives the update on the topic. Once the ions are separated, they are collected and detected in ion collector chamber. Most of the ion-pair spectrophotometric assay methods published in pharmaceutical field are based on UV-Vis molecular absorption. Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been freshly adapted for the recognition of whole microorganisms from their colonies on media or directly from cultures in blood and urine. The mass analyzer tube is the most important part on which a range of the mass spectrometer depends. Then, the signal is transferred to a data collection system for data investigation. © 2017 The Author(s). Fragmentation pattern is also an important component of mass spectra from which qualitative analysis of compounds can be done, and it is also useful in elucidation of structural arrangement of compound. A liquid chromatographic thermospray tandem mass spectrometric method was developed for quantitative analysis of some drugs having hypnotic, sedative and tranquilizing properties, that is, benzodiazepine, thioxanthene, butyrophenone, methadone and diphenylbutylpiperidine in whole blood. For its most popular model, the electron impact ionization with magnetic sector analyzer, the sample under investigation is converted into vapor phase and bombarded with electrons having energy sufficient to knock out one electron from it (>10 eV) to produce a positively charged ion called molecular ion or parent ion which is denoted by M+. The first mass spectrometer was developed in 1912 by J.J. Thompson. Regulatory demands also place “evidence of control” requirements on the composition and stability of the pharmaceutical products, and thereby the proof data associated with this process. This study is used to measure metal in the low concentration. Uttam Singh Baghel, Atamjit Singh, Deeksha Singh and Manish Sinha (December 6th 2017). Various examples from the literature support the present application. There are some rules which are employed in interpretation of mass spectra in structure elucidation process. Surface-enhanced Raman spectroscopy (SERS) is a sensitive analytical tool used in the pharmaceutical field in recent years. In the fast-developing fields of pharmaceutical research and industry, the implementation of Raman spectroscopy and related technologies has been very well received due to the combination of chemical selectivity and the option for non-invasive analysis of samples. Drug metabolic reactions can be divided into two parts: 1. It does this by diffracting the light beam into a spectrum of wavelengths, detecting the intensities with a charge-coupled device, and displaying the results as a graph on the detector and then on the display device. Brief introduction to this section that descibes Open Access especially from an IntechOpen perspective, Want to get in touch? The following examples from the literature support the present application of mass spectroscopy. The United States Pharmacopeia (USP) defines absorption spectroscopy as “the measurement of an interaction between electromagnetic radiation and the chemicals, or atoms, of a chemical substance.”. The analysis of sulfated heparin-like glycosaminoglycan oligosaccharides was done with the help of tandem mass spectroscopy (MS/MS) using quadrupole ion trap mass spectrometer and quadrupole orthogonal acceleration time-of-flight mass spectrometer, and their fragmentation pattern was also studied. Hydrogen deficiency index is also called unsaturation index which gives the information about the number of π-bonds and/or rings present in a molecular structure. A library of compounds were analyzed using mass spectra data collected by DART-MS operated in switching mode at 20, 60 and 90 V settings. Another similar study revealed a method for determination of amino acid sequence of fractions of peptides from apolipoprotein B by tandem mass spectrometry. Interpretation of hydrogen deficiency index: If hydrogen deficiency index is one, there must be one double bond or one ring present in the structure. We are IntechOpen, the world's leading publisher of Open Access books. For example, the particle size and distribution may be critical to the functionality of the drugs, and a high degree of quality control of the dissolution process is required. MALDI-MSI can be used for direct analysis of homogeneity of the active drug compound throughout the excipients contained in tablets. Custom-designed isotopic clusters resulting from the mixture of natural and synthetically enriched isotopes can greatly facilitate the detection and identification of metabolites. Hydrogen atoms in actual molecular formula of compound = 6. Mass spectrometry is a very sensitive technique which can analyze even minute quantities of the molecule. By making research easy to access, and puts the academic needs of the researchers before the business interests of publishers. Since pharmaceutical labs have so many uses for bench top spectrophotometers, these instruments must be versatile, accurate and easy to use in a variety of ways. This has contributed to the use of the spectroscope successfully in the detection of many of organic compounds, aromatic numerous active substances in drugs in the field of research chemicals, biochemical, and medical analysis of organic compounds.