Compared with other techniques, mass spectroscopy is only the technique for molecular weight determination, through which we can predict the molecular formula. Surface-enhanced Raman spectroscopy (SERS) is introduced as a particularly promising tool in this context. In the ion generation chamber, neutral sample molecules are ionized and then accelerated into the mass analyzer tube. In this technique, a portion of an isolated colony is loaded in the instrument and the comparison of spectrogram is done to a library by a proprietary algorithm to identify the organism. The amount of the actual drug can be very small and hence there is a need for highly sensitive and specific techniques for quantitative and qualitative analysis. MALDI-MSI can be used for direct analysis of homogeneity of the active drug compound throughout the excipients contained in tablets. The tandem triple quadrupole mass spectrometer equipped with an electrospray ionization source was used in the study [50]. After specific needed corrections, compare molecular formula of unknown compound with the formula of saturated hydrocarbon. Sometimes greater degree of sensitivity is required when analyte quantity is too low and mass spectroscopy due to its higher sensitivity marks a valuable place in clinical analysis [24]. It is generated due to loss of kinetic energy of ion during acceleration from ionization chamber to analyzer tube. The mass analyzer tube is the most important part on which a range of the mass spectrometer depends. 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]. It shows promising results in its ability to visualize the drug and excipients distribution in pharmaceutical formulations such as tablets, creams and ointments. Base peak: It is the most intense peak of the mass spectrum. We share our knowledge and peer-reveiwed research papers with libraries, scientific and engineering societies, and also work with corporate R&D departments and government entities. These recent hyphenated technological developments of the technique have significantly improved its applicability in pharmaceutical and biomedical analyses. In forensic studies, the use of mass spectroscopy is becoming significant because of increase in the demand to investigate use of illegal drugs through analyzing body fluids and tissues. Determination of 11-nor-9-D-tetrahydrocannabinol-9-carboxylic acid (THC-COOH) in urine [41], alfentanil, fentanyl and its derivatives with other opioid drugs like morphine, buprenorphine, codeine, heroin, methadone, naloxone, naltrexone, tramadol, pentazocine, pethidine and others in hair [42] has been done by LC–MS and LC–MS/MS. Of the species-level identifications, 95.1% matched conventional identifications. Mass spectrometer mainly consists of following components: The inlet system transfers the gaseous form of sample into the vacuum of the ion generation chamber of mass spectrometer. A new technique was developed for the identification of proteins on tissue using tryptic digestion followed by matrix-assisted laser desorption/ionization imaging mass spectrometry with tandem mass spectrometry analysis. Implementation of mass spectroscopy in clinical laboratory resulted in significant advancements. The instrument has now a wide range of applications in pharmaceutical (drug discovery, pharmacokinetics, drug metabolism), clinical (neonatal screening, hemoglobin analysis, drug testing), environmental (water quality, food contamination, pollutant determination), geological (oil composition, hydrocarbon fraction determination in petroleum industry), metallurgy (determination of rare earth metals and metals at ppq (parts per quadrillion)), sports (dope test … Analysis of molecular bond strengths 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. Hydrogen atoms in actual molecular formula of compound = 6. Hydrogen deficiency index is 4, because four pairs of hydrogen atoms are required to saturate the compound. APPLICATIONS OF UV SPECTROPHOTOMETRY IN PHARMACEUTICALS • Qualitative analysis through spectrophotometric methods achieves fast and accurate results using only small sample quantities. Then, the signal is transferred to a data collection system for data investigation. 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. These are: Nitrogen rule: Nitrogen rule gives very useful clue about the presence or absence and number of nitrogen atoms. Uttam Singh Baghel, Atamjit Singh, Deeksha Singh and Manish Sinha (December 6th 2017). Bile acids have many vital physiological functions like lipid absorption and cholesterol homeostasis. How? Pharmaceutical Applications (UV–vis) Of the four spectrophotometric techniques described in this chapter, currently the number of UV–vis procedures in use in the pharmaceutical industry probably accounts for more than all of the other three, that is, NIR, mid-IR, and fluorescence, combined. In atomic absorption spectrometry for example. 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]. A method based on MALDI-FTICR for imaging of olanzapine in kidney and liver as well as imatinib in glioma was described [30]. The presence of an analyte gives a response which can be assumed to be proportional to the concentration. 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. Combination of TOF with one (Q-TOF) or two quadrupoles (Qq-TOF) is emerged as hybrid mass spectrometers that are able to cover unlimited mass range with high scan rates up to 106 u/s and high resolving power. The characterization of polyisobutylenes was done by various mass spectrometry techniques like tandem mass spectroscopy with MALDI-TOF and ESI-QIT. However, sequencing of underivatized peptides as in fast atom bombardment mass spectrometry (FABMS) is also employed. 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. Mass spectrometry (MS) is an advanced technique for determining the molecular weight of a compound. By optimization, the cost of operation reduces to one-tenth that of conventional method with automated biochemical testing platforms. Hydrogen deficiency index is 1, because one pair of hydrogen atom is required to saturate the compound. A simplified method was developed for clinical diagnosis of organic aciduria with gas chromatography–mass spectrometry (GC–MS) using quadrupole mass spectrometer. HeadquartersIntechOpen Limited5 Princes Gate Court,London, SW7 2QJ,UNITED KINGDOM. The first mass spectrometer was developed in 1912 by J.J. Thompson. A UV/Vis spectrophotometer may be used as a detector for HPLC. For many years, GC–MS has been used but LC–MS has also been used for qualitative analysis of bile acids. 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]. This method has important advantages over others because of the high specificity, sensitivity and selectivity of tandem mass spectrometry [31]. To date our community has made over 100 million downloads. In this, triple quadrupole mass spectrometer along with LSI-MS was employed [23]. The following examples from the literature support the present application of mass spectroscopy. The urine samples were analyzed from patients, and acids were identified like methylcitric acid, margaric acid and glutaric acid [27]. This segment separates generated ions, either in space or in time, according to their mass-to-charge ratio (m/e). A direct analysis in real-time ion source coupled with a time-of-flight mass spectrometer (DART-MS) method for screening of pharmaceutical formulations was developed. New techniques like MALDI and tandem mass spectroscopy are also in trend [18, 19]. A Swiss study has done a comparison between MALDI-TOF MS system and conventional methods for the identification of 1371 routine bacteria and yeast isolates. For example, the detection and identification of ribavirin metabolites in rats was done with the aid of stable isotope labeled drug [49]. APPLICATIONS OF IR SPECTROSCOPY Infrared spectroscopy is widely used in industry as well as in research. Similarly, it can also be used for detecting the purity profile of active pharmaceutical ingredients (API), that are, MK-0969, an M3 antagonist; MK-0677, an oral-active growth hormone secretagogue and API-A, a cathepsin K inhibitor. Likewise, the level of antitumor drug SCH 226374 was determined in mouse tumor tissue using MALDI-QqTOF mass spectrometer. By Uttam Singh Baghel, Atamjit Singh, Deeksha Singh and Manish Sinha, Submitted: December 18th 2016Reviewed: August 22nd 2017Published: December 6th 2017, Home > Books > Spectroscopic Analyses - Developments and Applications. In forensic study, sample is in minute quantity; therefore, high sensitivity is required for analysis. This opened the new horizons of its applicability. Mass spectroscopy coupled with gas chromatography emerged as an indispensable tool in forensic field as well as LC–MS has also wide utility in forensic study. A triple-stage quadrupole mass spectrometer was used in the analysis at a very low detection limit of 0.05–0.5 ng/ml [39]. Much of the need for accurate optical property measurements stems from the need to control the purity and dose of the drugs, in the development, manufacturing, and quality control of the product, and therefore at the beginning of the chapter, we discuss an overview of these processes. They used MALDI-TOF for their study [29]. Hydrogen atoms in actual molecular formula of compound = 4. These changes can be accurately measured by mass spectrometer. Peptides are converted into amino alcohols which are volatile in nature. This technique can precisely identify even those bacteria which are difficult by conventional methods and that day is not far away when this technology will complement the conventional microbiologic identification methods. This paper delineates FTIR as a quantitative tool used now-a-days and other analytical applications in pharmaceutical and allied areas. Mass spectroscopy can also be used for the investigation of bile acids in biological fluids. Mass spectroscopy is widely used for detection of impurities in samples. ASSAY OF SODIUM, POTASSIUM AND CALCIUM IN BLOOD SERUM AND WATER Help us write another book on this subject and reach those readers. 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]. Mass spectrometry is a very sensitive technique which can analyze even minute quantities of the molecule. It is also a noninvasive tool that permits in vivo studies in humans. The primary structure was determined by multistage mass spectrometric analysis, the presence of specific functional groups (e.g., OH or OCH3) was confirmed, and also differentiation between isomeric functional groups was done [17]. By Tünde Jurca, Eleonora Marian, Laura Graţiela Vicaş, Mariana Eugenia Mureşan and Luminiţa Fritea. The Use of Spectrophotometry in the Pharmaceutical Industry. A new procedure was revealed which enabled selective sequencing and detection of serine-, threonine- and tyrosine-phosphopeptides at very low level of femto mole in protein digests with electrospray mass spectroscopy (ES-MS) using quadrupole mass spectrometer [22]. Therefore, base molecular formula will be: Hydrogen atoms in predicted base molecular formula = 14. Isotopic peaks: Isotopic peaks are often seen in the mass spectrum due to the presence of isotopes. The elucidation of impurity structure was made by utilization of LC–MS using quadrupole ion trap mass spectrometer equipped with an electrospray ionization or an atmospheric pressure chemical ionization (APCI) interface [35]. In some cases, instruments have identified only one organism without indicating the presence of others. 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]. Thus, it is an important tool for structure elucidation of unknown compounds. These are usually one or two mass units higher or lower than the ion peak. 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. This study suggested the use of tandem mass instruments like Q-TOF and metal cations in mass spectroscopy of heparin-like glycosaminoglycan oligosaccharides [13]. 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. For group VII elements (F, Cl, Br, I): The removal of one hydrogen atom is required with each added element. For example, it … C6H6 has six carbon atoms. Mass spectrum is produced in the form of bar graph which is interpreted by using the following peaks. Several phytoconstituents are volatile and thermolabile, and they can be analyzed by electrospray ionization (ESI) and matrix-assisted laser desorption ionization (MALDI). 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. There are some rules which are employed in interpretation of mass spectra in structure elucidation process. Additional peaks can be observed due to impurities in the sample and … Spectroscopic related Applications. For group V elements (N, P, As, Sb, Bi): Addition of one hydrogen atom is required with each added element. It’s based on principles of collaboration, unobstructed discovery, and, most importantly, scientific progression. 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. Organic acidurias are an inherited disorder of metabolism in man, and gas chromatography coupled with mass spectroscopy is used to define an organic aciduria involving isovaleric acid. Surface-enhanced Raman spectroscopy (SERS) is a sensitive analytical tool used in the pharmaceutical field in recent years. Typical spectrophotometry applications are the measurements of nucleic acids, proteins and bacterial density. For example, the H/D exchange method was used for the drug metabolism studies of denopamine and promethazine in which N- or S-oxide was easily distinguished from the hydroxylated metabolites. Detection of Impurities UV absorption spectroscopy is one of the best methods for determination of impurities in organic molecules. This study has been used in many applications related to the spectroscopy field. Similarly, a fast and sensitive liquid chromatography–tandem mass spectrometry method was developed for simultaneous determination of acetaminophen and its glucuronide and sulfate metabolites (APAP-GLU and APAP-SUL) in small plasma volumes. SERS keeps all the advantages of classical Raman spectroscopy while being is more sensitive allowing its use for the detection and the quantification of low-dose substances contained in pharmaceutical samples. By continuing you agree to the use of cookies. From Beynon table, one can predict the possible elemental arrangement or composition of particular mass and determine the molecular formula of compound. Indeed, it is suitable for analysis of solid, liquid, and biotechnological pharmaceutical forms. The cross-linking/MS was used as an integrated structure analysis tool for large multi-protein complexes [21]. Therefore, base molecular formula will be: Hydrogen atoms in predicted base molecular formula = 6. There is dramatic amplification in interest and implementation of clinical mass spectrometry for testing of vitamin D. LC–MS/MS method enables to distinguish between vitamin D2 and vitamin D3 and also provides information on the vitamin D epimeric form, both of which are not currently possible with existing immunoassays. The spectrophotometer is utilized for research and data evaluation in different scientific fields. Spectrophotometry journals cover varied fields like Chemistry, Physics, Organic Chemistry, Material and Chemical Engineering and Clinical Applications. Glancing at the recent advances, Fourier Transform Infrared Spectroscopy sciences. Matrix-assisted laser desorption ionization-Fourier transform ion cyclotron resonance (MALDI-FTICR) is also an efficient technique for imaging of drugs and metabolites in tissue. The results coincide with the results obtained by the GC–MS technique. Newer techniques, such as laser-induced breakdown spectroscopy (LIBS) and Laser Ablation ICP-MS (LAICP-MS) are also beginning to see wider applications in the analysis of elements in the pharmaceutical industry.This article will provide a perspective regarding the various applications of atomic spectroscopy in the analysis of metals and metalloids in drug products, active pharmaceutical … New methods and instruments in mass spectroscopy are developed at a very high rate. Intensity of the peak depends on the natural abundance of isotopes. This is used for the confirmation of proposed fragmentation pattern of a molecule. Applications Spectroscopy is used as a tool for studying the structures of atoms and molecules. *Address all correspondence to: drusb1985@yahoo.com, Spectroscopic Analyses - Developments and Applications. The instrument has now a wide range of applications in pharmaceutical (drug discovery, pharmacokinetics, drug metabolism), clinical (neonatal screening, hemoglobin analysis, drug testing), environmental (water quality, food contamination, pollutant determination), geological (oil composition, hydrocarbon fraction determination in petroleum industry), metallurgy (determination of rare earth metals and metals at ppq (parts per quadrillion)), sports (dope test of drugs in athletes), forensic (poison and drug metabolite determination) and biotechnology (proteins, peptide analysis) like fields. It shows promising results in its ability to visualize the drug and excipients distribution in pharmaceutical formulations mass analyzer is. 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