An Overview: LC-MS as Tool of sample Extraction and Quantification in Bioanalytical Laboratories
Pramod K.*, Amar Deep A., Pooja K., Mahendra Singh A.
Department of Pharmaceutical Analysis and Quality Assurance, Laureate Institute of Pharmacy Kathog, Jawalaji
*Corresponding Author E-mail: gargpramod081@gmail.com
ABSTRACT:
LC-MS/MS is the hyphenated techniques which is used for the identification and quantification of the organic compounds in bioanalyitical laboratories. LC-MS instrument is basically combination of liquid chromatography unit and mass spectrometer to achieve dual benefits. In other hand, LC-MS/MS is Liquid chromatography with two mass spectrometer units specifically analyzers for better resolution. LC-MS/MS is widely used for separation of biological samples of different origins like protein, urine, blood, saliva, tissue. The prefence are mainly due to its specificity, precision and accuracy. In this review article, we will discuss the use of this hyphenated systems in analysis of protein, oxysterols, stratum corneum and metabonimics. Sample preparation techniques such as protein precipitation, liquid-liquid extraction, and solid phase extraction and affinity techniques and effective analysis by LC/MS/MS. This approach is also preferred for the separation of antibodies, proteins and enzymes from the biological matrix.
KEYWORDS: LC-MS/MS, Protein, Oxysterols, Metabonimics and Stratum corneum.
INTRODUCTION:
Bioanaytical laboratories carry out the quantitative and qualitative analysis of xenobiotic and pharmaceuticals in the biological system. Xenobiotic are broad term and refer to the drugs and their metabolites, endogenous molecules, macromolecule, proteins, DNA, giant molecule and toxicants. A bio analytical method is the set of procedure concern with different processing, different techniques which utilizes analytical principles to isolate and estimate the chemical entities from biological sample or matrix.
Recent advances in bioanalytical techniques utilize hyphenated systems to get desired result with accuracy, precision and short span of time with small sample size. The common technique are LC/MS/MS, GC/MS, and LC/NMR etc. On the other hand, the biological sample consist of saliva, proteins, blood, urine etc. The provision of selective and sensitive bio analytical strategies should be necessary to generate of reliable information on pharmacological medicine, bioavailability and bioequivalence of medication.(1-2)
Quantitative determination of medicine and their metabolites in biological fluids is crucial throughout drug discovery and development. Liquid chromatography mass analysis (LC/MS) permits the analysis of advanced mixture of little molecules in biology drugs and drug molecular characterization of sample in environmental chemistry and combinational chemistry among several alternative application. LC-MS also widely used in molecular pharmacognosy once it involves the ingredient distinction within the aspects of constituent biological and phytochemistry. It paves path for discover of drug from natural origin and its characterization. The most vital issue that needs to be thought of is the way to create the most important distinction of active ingredients in plant cells between the check cluster of plants and controlled ones.(3-6)
SAMPLE PREPARATION METHOD FOR LC/MS/MS:
The sample preparation is to be easy at low price and permit matrix reduction with the choice to concentrate the analytes of interest but it need to be high degree of accuracy in the preparation of sample even minute particle easily determined so the impurities in the drug or sample easily detected. LC/MS samples containing non-volatile or large compounds square measure generally ready for mass qualitative analysis (MS) analysis by 1st undergoing liquid activity (LC) separation than mass analyser. This is a necessary step within the ultimate isolation and identification of the target analyte from among of thousands of alternative compounds and contaminants. The sample preparation for the LC/MS easy but need to pure compound. Liquid-liquid extraction contain a long history for the preparation of the sample and alternative technique are assessable that have supplanted in some cases but this system still has value for the preparation. Another technique is protein precipitation technique used for the sample preparation. more recently technique usually known as solid-phase extraction (SPE) used. Most current applications of sample preparation for LC/MS use some variant of those techniques. Another vital sample-preparation technique is critical fluid extraction (SFE) that has been used in biological and particular, especially environmental sample preparation.(7-9)
Protein precipitation:
Liquid–liquid extraction (LLE):
Liquid–liquid extraction (LLE) also known as solvent extraction and partitioning. Liquid–liquid extraction has been used in sample preparation work flows for several years and involves the partitioning of analytes from an aqueous bio fluid into a water immiscible organic solvent supported polarity. It offers variety of advantages for LC-MS/MS assays because it allow to increase the concentration of analytes and reduces the matrix component that increase selectivity. This multi-step process is comparatively labour intensive requiring the partitioning of the analytes into the organic solvent separation of the organic and aqueous layers evaporation solvent and reconstitution of the analytes during a solvent mixture that's miscible with the LC mobile phase. In some cases, as many as three immiscible layers may form due to the various densities of the solvents (shown in figure 1). Many factors have an effect on the recovery and property of the analytes from the solution, as well as analyte solubility and pKa, resolution hydrogen ion concentration, and ionic strength. After separation of the immiscible liquids by activity the organic layer containing the extracted associate degreealytes is removed targeted to xerotes and reconstituted in an applicable solvent foreseeably the HPLC mobile phase for LC/MS analysis.(14-15)
The solvent selection is predicated on the based on
polarity polar solvents extract polar analytes most of the polar component used
so the polar solvent used to extract polar compound. Consequently LLE can’t be
specified analyte because the solvent will extract all molecules from the
matrix (endogenous and exogenous i.e. xenobiotic) with similar chemical
properties all the polar component which present in xenobiotic.This
type of technique is employed to extract group or families of molecule as well
as benzodiazepines and antidepressants for the screening of artificial cannabinoids.One problem in liquid-liquid extraction is
minimizing exposure of the analytes to potentially adsorptive surfaces.
Exposing analytes to silanol group on silicon oxide surfaces found in
solid-phase extraction techniques will cut back recovery.The
silanol group need to solid phase for extracting of analytes.This
result is less clearly all over liquid-liquid, extraction however chemisortive losses happen throughout the solvent removal
or "blowdown" step following extraction once the analyte is allowed
to create a dry residue on the within surface of the container. In addition
aerosol action/physical changes with the addition of alcohol losses throughout
the blowdown step if the analyte forms particulates or is comparatively
volatile. Although impractical not concentrating the extraction solvent layer
to condition will prevent these potential issues.The
final reconstitution solvent necessary to dissolve the extract fully and
compatible with the initial HPLC mobile phase. When all of these
conditions are met, liquid-liquid extraction provides excellent results.(16-22)
(Fig.1)
SPE has its commercial roots within the late 70s since then it's become a standard and effective technique for extracting analytes from advanced samples. The SPE used since 70s because its efficient result and now it’s used to extracting. Solid phase Extraction (SPE) may be a powerful technique for sample preparation. It is used in wide range of application areas, including environmental analyses, pharmaceutical and biochemical analyses chemistry, food analyses, agricultural and used in also other field. Solid-phase extraction is one amongst the foremost common types of sample preparation in current use. It is usual format involves introducing a liquid sample to an extraction cartridge during a small syringe-shaped container. The cartridge contains a solid phase capable of extracting the analytes of interest and retaining them on the solid phase. The analyte is thus removed from a ‘dirty’ matrix then eluted from the solid phase and injected into a GC or an HPLC. SPE utilises a liquid-solid extraction separation principle during which an outsized particle sized sorbent is sealed into a small chromatographic column. The required analytes are then selectively off from the column either before or after removal of interfering compounds. The interfering compound are the other compound like primary metabolites sometimes also secondary metabolites. The main objectives of SPE are removal of interfering matrix components and selective concentration and isolation of the analytes of interest. It allows GC, HPLC and other chromatographic methods to better qualitative and quantitative analysis. The principle of SPE is analogous to it of liquid-liquid extraction (LLE), involving a partitioning of solutes between two phases. However rather than two immiscible liquid phase as in LLE, SPE involves partitioning between a liquid (sample matrix or solvent with analytes) and a solid (sorbent) phase. The sample treatment technique is allow the concentration purification of analytes from solution by means of sorption on a solid sorbent and purification of extract after extraction the main purpose is to purification of analytes for the better and accurate result. The common method is to load a solution into the SPE solid phase, wash the undesired components, and then wash off the preferred analytes with another solvent into a series tube. SPE have many advantage in comparison with in more common sample preparation technique (e.g. liquid-liquid extraction) such as excessive recoveries of the analyte concentration of analyte highly purified extract capacity to simultaneously extract analyte large range ease of automation compatibility with instrumental analysis and reduction in natural solvent.(23-34)
General steps of solid- phase extraction shown in figure 2.
(Fig.2)
Affinity techniques coupled with LC/MS:
A high degree of molecular selectivity can be completed with affinity chromatography and affinity extractions. This method is most selective and used to separate the antibodies, proteins and enzymes from the biological matrix the separation of compound and analytes depend upon the affinity towards the solvent. It is primarily based on biological interactions between two molecules like enzyme substrate, receptor and ligand or antibody and antigen like antigen-antibodies reaction. When a mobile phase containing combination of proteins/ antibodies/enzymes are surpassed through the stationary phase only the specific protein binds to its respective ligand in the stationary phase the specific antibodies bind with specific antigen. This protein later can be extracted by using changing the ionic strength or pH. These techniques are based totally upon molecular recognition and can isolate and concentrate specific analytes, from complex sample matrices. This technique give a high degree of purification of a targeted analyte is viable in a single step from large volumes of sample. Combining immune affinity extraction (IAE) and ultrafiltration with MS provide an effective high quality method to analysing complex samples by exploiting the advantages offered by each technique. A practical method is to couple IAE on-line with LC/MS or to prepare samples off-line using ultrafiltration mixed with column-switching methods. IAE minimizes pattern preparation techniques, selectively concentrates analytes and LC/MS provides a quick and very selective detection method for captured analytes when eluted from the affinity medium. When IAE methods are used, analytes from a sample matrix might also be detected through LC/MS/MS monitoring of selected precursor and product ion pairs to supply sensitivity enough for ultra-trace quantitation.(35-36)
Fig. 3: APPLICATION OF TANDEM MASS SPECTROMETRY:
Analysis of Protein:
Comparing two or more complex proteincombinations using liquid chromatography mass spectrometry (LC-MS) requires more than one analysis steps to locate and quantitate herbal peptides within a single test and to align and normalize finding throughout multiple experiments. An open-source application comprising algorithms and visualisation tools for the analysis of more than one LC-MS experimental measurements.The platform integrates novel algorithms for detecting signature of herbal peptides a single LC-MS measurement and combine multiple experimental measurements into be peptide array which may two the use of analysis tools traditionally utilized to genomic array analysis. The platform support quantitation through each label-free and isotopic labelling approaches. The software program implementation has been designed so that many key factors can also be easily replaced making it beneficial as a work bench for integrating. As developed the algorithms for ms inspect, made a several options based totally on know-how of fundamental standard and routine visible inspection of data. For example of the many quality measures should use to enhance peptide location, chose to examine resulting distribution to an easy poisson approximation to identify herbal isotopic shapes. We observed the poisson approximation carried out as well as the more computationally intensive approach but was once more accurate when used outdoor the range they considered. Also, when assigning a volume to a located peptide selected to use only the maximum intensity of its isotopes as a substitute than summing intensities over all of its identified isotopes. Simply summing specific components every measured with one of a kind precision need to end result in decreased reliability overall. Thus even though we provide a mechanism to combine more than one charge state by summing their intensities we do not recommend doing so until better methods for combining multiple charge states are developed. It is unlikely that any single implementation of the entire pipeline outlined will include the satisfactory approach at every step, and continued research needed for each of the individual elements. The excellent step forward may also come from integrating and comparing the exclusive open source algorithm implementations. The MS inspect application has been designed to allow substitute of many individual components with alternate, competing methods, and like other methods with different algorithms, the source code has been made available in order to foster the synthesis of the high-quality components into one or more platforms.(37-42)
Analysis of Oxysterols:
These oxysterols are important molecules for preserving lipid homeostasis in the body.7a-Hydroxycholesterol is a product of CYP7A1, which is the rate-limiting enzyme in the basic bile acid biosynthetic pathway. 27-Hydroxycholesterol, 24S-hydroxycholesterol, 4b-hydroxycholesterol 22R-hydroxycholesterol, and 24S, 25-epoxycholesterol are high quality endogenous ligands of the nuclear receptors liver X receptor a (LXRa) and LXRb.In addition, 27hydroxycholesterol, 25-hydroxycholesterol, and 24S, 25-epoxycholesterol are known to down regulate the cholesterol biosynthetic pathway most likely by blockading the processing of the sterol-regulatory element binding protein. This approach is primarily based upon a stable isotope dilution technique by mean of liquid chromatography-tandem mass spectroscopy (LC-MS/MS). After alkaline hydrolysis of human serum (5 ml) or rat liver microsomes (1mg protein), oxysterols had been extracted, derivatized into picolinyl ester and analysed through LC-MS/MS the use of the electrospray ionization mode. The detection limits of the picolinyl esters of 4b-hydroxycholesterol, 7a-hydroxycholesterol, 22R-hydroxycholesterol, 24S-hydroxycholesterol, 25-hydroxycholesterol, 27-hydroxycholesterol, and 24S, 25-epoxycholesterol had been 2–10 fg on-column.(43-45)
Analysis of Stratum corneum:
Lipids Ceramides in the top layer of the skin, the stratum corneum (SC) play a key function in the skin barrier function. A novel fast and robust LC-MS approach is that permits the separation and analysis of all known human stratum corneum lipids ceramides subclasses using only limited pattern preparation. Besides all 11 recognized and identified subclasses, a 3D multi mass chromatogram indicates the presence of different lipid subclasses.Using LC/MS/MS with an ion trap system a Fourier transform-ion cyclotron resonance system, and a triple quadrupolesystem, we had been capable to identify one of these lipid subclasses as a new lipids ceramides subclass: the ester-linked hydroxy fatty acid with a dihydrosphingosine base (Lipids Ceramides. The identification of a lipid ceramides subclass, additionally describe the applicability and robustness of the developed LC/MS technique through analyzing three (biological) stratum corneum samples: stratum corneum from human dermatomes skin human SC obtained by tape stripping, and stratum corneum from full thickness pores and skin explant. All three biological sample showed all known stratum corneum subclasses and mild differences had been discovered in lipids ceramides profile.(46-48)
Lipids ceramides classification:
The lipids ceramides consist of either a sphingosine (S), a phyto-sphingosine (P), a 6-hydroxy sphingosine (H) or a dihydrosphingosine (dS) base. This base is chemically linked to either a nonhydroxy fatty acid (N), ἁ -hydroxy fatty acid, or an esterified ὠ-hydroxy fatty acid. 11 distinct lipids ceramides subclasses, viz., lipids ceramides denoted through [NS], [NdS], [NP], [NH], [AS], [AdS], [AP], [AH], [EOS], [EOP], and [EOH](48-50)
Analysis of Metabonimics:
Metabolomics objectives at identification and quantitation of small molecule involved in metabolic reactions. LC-MS has enjoyed a developing popularity as the platform for metabolomic studies due to its excessive throughput, soft ionization, and precise coverage of metabolites. The success of LC/MS based metabolomic study often depend on multiple experiment, analytical, and computational steps. The identification of metabolites is the current bottle-neck in LC-MS-based metabolomic studies. Although it is usually easy to measure the exact mass of molecular ion detected in LC-MS experiment, mass data is regularly not adequate to completely signify its structure and identify it as a unique biochemical activity. Although novel metabolites continue to be discovered many of the metabolites face in practice have already been discovered and recognized in some other studies. The collection and utilization of these “known unknowns” pose fundamental challenges for computational and informatics tools. This is in phase because the data is regularly scattered in special sources, in various formats, and with spectra acquired under different condition. In addition to information collection, multiple steps, are required to completely utilize the records embedded in LC-MSD data. Automated acquisition of high-quality MS/MS spectra is needed to increase the throughput of metabolite identification. Improved in-silico fragmentation model of metabolites are needed, which consider complex ion-molecular interactions encountered in metabolites fragmentation. LC-MS/MS spectral libraries for metabolites, continue to evolve and expand for improved metabolome coverage. In addition carefully designed experiments and suitable spectral matching algorithms are desired to make sure spectral libraries from different laboratories and instrument are transferable. The metabolome is the set of small molecule mass natural compound located in a given biological media. Metabolomics refers to the untargeted quantitative or semi-quantitative analysis of the metabolome and is a promising device for biomarker discovery. MS and chromatography have been substantially developed in the previous few many years and hold an individual position in qualification and separation science. The advancement of each HPLC and MS has contributed significantly to metabolomics analysis. MS and HPLC are normally used for compound characterization and obtaining structural information; in the field of metabolomics, these two analytical method are often combine to signify unknown endogenous or exogenous metabolites present in complex biological samples. With HPLC coupled to MS, there is no need to derivatize compounds prior to analysis. LC-MS method have been develop using a smooth ionization approach making MS more robust for daily use. It should be mentioned that LC-MS can provide a list of m/z values, retention times and an estimation of relative abundances of identified metabolites that are not clearly identified.High-resolution and reproducible LC/MS measurement sets up the basis for subsequent information processing and multivariate record analysis.Large-scale metabolomic technologies based on LC-MS are increasingly gaining interestfor their use in the analysis of human disease. Development of robust, sensitive, and reproducible diagnostic test for understanding diseases is a global manage program. Due to its sensitivity and quantitative reproducibility LC-MS based totally metabolomics is a powerful method to this problem. An LC-MS metabolomics-based diagnostic provides a fundamental tool and has the potential to monitor the progression of onchocerciasis. LC-MS based totally nontargeted metabolomics has been completely tested, validated, and utilized to screen/identify and validate novel metabolic biomarkers for epithelial ovarian cancer; six key-metabolites had been considered as potential biomarker candidates, geared up for early stage detection. LC-MS technique was effectively applied for metabolomic analysis of hydrophilic metabolites in a wide range of biological samples. Classification separation for metabolites from different tissue was globally analysed through PCA, PLS-DA and HCA biostatical method. A total number of 112 hydrophilic metabolites were detected within eight min of running time to obtain a metabolite profile of the biological samples. LC-MS technique for targeted multiple response monitoring has become a useful tool for the analysis of lots of polar metabolites in a complex sample. Targeted bile acid analysis using LC/MS metabolomics verified increased levels of conjugated or unconjugated bile acids and can allow the different-different types of hepatobiliary toxicity. (51-56)
Analysis of Amino Acid:
The amino acid have unique fragment ion produce when it introduce into mass spectrometry which analyse by MS/MS. Amino acid phenylalanine tyrosine, leucine alanine leucine, alanine, valine, and methionine have different fragment ion. The ionisation of amino acid can be enhanced by the esterification of free carboxylic acid. The mass of a protonated molecule is denoted as (M+H) +. H (1 Da) it is represents the proton which associates with basic functional groups containing nitrogen, such as amines and note the charge on an amino acid is 1. The horizontal axis represents the mass spectrum (m/z, mass/charge) which generated by MS/MS. The vertical axis represents the number of ions detected (either absolutely or as a percentage relative to the largest amount detected relative intensity). The amino acid analysis by MS/MS which help to identify the amino acid disorder. Phenylketonuria, Maple Syrup Urine Disease, Homocystinuria, Tyrosinemia and Basic Amino Acids.
Phenylketonuria:
The MS/MS is capable to identifying and quantifying the amino acid. The phenylketonuria is characterised by the deficiency or the phenylalanine hydroxylase. This enzyme used for the conversion of phenylalanine to tyrosine, the accumulation of the phenylalanine and concentration of tyrosine is decreased. In the MS/MS spectra the phenylalanine mass is high and tyrosine is less.(57-58)
Applications in Endocrinology:
The tandem mass spectrometry has been recognized as a primary methodology for the accurate analysis of endogenous steroid hormones in biological samples. A diagnostic testing depends on the appropriateness of the utilized markers of diseases. The liquid chromatography–mass spectrometry (LC–MS) methods for quantitative analysis of endogenous steroids use triple quadrupole mass spectrometry (MS/MS). Data collected during the LC–MS/MS analysis contain three dimensions: retention time, m/z of the precursor ion, and m/z of the product ions. The data collected during the analysis represents properties of the molecules, structure and molecular weight. The multiple-reaction monitoring used to detect the quantitative analysis of the sample. The multiple-reaction monitoring mode of operation is highly selective and sensitive because the mass analysers transmit only ions, characteristic of the target analyte, and remove most of the chemical noise. This combination with multiple-reaction monitoring technique is achievable in clinical diagnostic laboratories. The various type of the endogenous steroid analysed example adrenal steroids, glucocorticoids, androgens, estrogens, ovarian steroid genesis, steroids in follicular fluid etc.(59-60)
Determination of Pesticides Fruits and Vegetables:
The use of pesticide in now days is common for the protection of food and maintained the quality of the food. The pesticide are toxic in nature used to kill the pest and insect. Most of the pesticides are volatile and thermally stable. Some pesticide are poor volatile and thermally not stable high polar compound these pesticide can be easily detected by the liquid and tandem mass spectrometry. This technique is powerful for the analysis of the residue of pesticide. The vegetable and fruits used to production of the baby food so the limitation of pesticide is less than 0.010mg/kg. The list of the pesticide which identified and quantified with this technique are, imidachloprid, trifloxystrobin, kresoxim-methyl, indoxacarb, fenothiocarb, furathiocarb, benfuracarb, fenazaquin, dimethomorph, fenpyroximate, hexythiazox, tebufenpyrad, tebufenozide, fenbuconazole, flusilazole, paclobutrazol, tebuconazole, tetraconazole, etofenprox, bromuconazole, fenhexamid, pyridaben, difeconazole, azoxystrobin.The extracts are analyzed by liquid chromatography–electrospray ionization tandem mass spectrometry (LC–ESI–MS–MS).(61-62)
Application of Liquid Chromatography-Tandem Mass Spectrometry in Forensic Toxicology:
The liquid chromatography-tandem mass spectrometry used in the forensic field for the identification and quantification of compounds. LC–MS–MS instruments work on based on various analytical principles to ionisation (e.g. electro- spray ionisation (ESI), atmospheric pressure photo ionisation (APPI) or atmospheric pressure chemical ionisation (APCI), matrix-assisted laser desorption (MALDI)) as well as detection (quadrupole, ion trap, time of flight and various of their combinations to tandem MS). Specificity plays an important role due to the limited separation power of liquid chromatography and the popularity of dirty matrices in the forensic toxicology field. This technique applied in forensic cases for the characterisation on compound in low concentration example of compound alprazolam, piritramide, dothiepine andcocaine etc. LC-MS in forensic science used to identification of the analytes at low concentration like drug abuse (LSD, cannabinoide, amphetamines)ethylglucuronide, antidepressants, ketamine, alkaloids, corticosteroidsandcyanide) amphetaminescocaine, THC, LSD, opiates explosives, pesticide, anabolic agents, benzodiazepines, neuroleptics or biogenic toxins (alkaloids, glycosides, amanitine).(63)
CONCLUSION:
The liquid chromatography is powerful technique is used for qualitative and quantitative analysis. The tandem mass spectroscopy is used for the identification of the molecular mass of the compound. When these technique combined each other the result is become more accurate. These tandem mass spectrometry techniques used for identification, analysis of the organic, biological compounds. The biological sample like protein, stratum corneum, oxysterols, metabolomics, amino acid etc. The sample preparation for LC-MS/MS by using liquid-liquid separation, solid phase separation, protein precipitation etc. The biological sample can be easily identified by using this powerful techniques.
REFERENCE:
1.
Ackermann BL, Berna
MJ, Murphy AT. 2002. Recent Advances in Use of LC/MS/MS for Quantitative
High-Throughput Bioanalytical Support of Drug Discovery. Curr
Top Med Chem. 2:53-66.
2. Maheshwari G, ShanthaKumari K, Abdul Rahaman S, Revathi S, Neeharika M. 2013 Review On LC-MS/MS In Bioanalytical Studies. World Journal of Pharmaceutical Research. A World Journal of Pharmaceutical Research. 2754-2780.
3.
Beckett AH and Stenlake GH. Practical Pharmaceutical Chemistry, Fourth
ed., CBS Publishers and Distributors, New Delhi, 2005.
4.
Patti GJ, Yanes O, Siuzdak G. Metabolomics:
The Apogee of the Omics Trilogy. Nature Reviews Molecular Cell Biology. 2012;
13(4):263–9.
5.
Cheng X, Hochlowski J, Current Application of Mass Spectroscopy to
Combinatorial Chemistry, Analytical Chemistry 2002-74(12):2679-90.
6.
Sharma BK.
Instrumental Methods of Chemical Analysis, Twenty Third Ed., Goel Publishing
House, Meerut, 2004.
7. Svec F, Huber CG. 2006 Monolithic Materials: Promises, Challenges, Achievements. Anal Chem 78(7):2100–2107.
8. Anderson, M. A; Wachs, T. Henion, J D. /. Mass Spectrom. 1997, 32,152-58. (7) Wu, Y.; Lii L Y-T.; Henion, J. D.J. Mass Spectrom. 196, 31,987-93. (8) Wu, Y; Zhao, J.; Henion, J.; Korfmacher, W. A; Lapiquera, M. P.; Lin, C-C.J. Mass Spectrom. .197, 32,379-87.
9. Taylor, L. Supercritical Fluid Extraction; John Wiley and Sons: New York, 1996.
10. C. Bylda, R. Thiele, U. Kobold nad D. A. Volmer, Drug test. Anal, 2013)
11. C. Bylda, R. Thiele, U. Kobold nad D. A. Volmer, Recent advancement in sample preparation techniques, 2014)
12. C. Ferreiro Vera., F. PriegoCopote and M. D. Luque de Castro, J Chromatogr. A, 2012)
13. J.
Carmichael and S. Brown, “The impact of phospholipids and phospholipid removal
on bioanalytical method performance”, Biomed. Chromatogr.
30, 710–720 (2016).
14. Covey, T. R.; Silvestre, D.; Hoffman, M. K.; Henion, J. D. Biomed. And Environ. Mass Spectrom.
.988, 15,45-56
15. G.
Hendriks, D.R.A. Ugesand J. P. Franke, J. Chromatogr. B: Anal. Technol. Biomed. Life Sci, 2007, 853,
234–241.
16. M.
Jemal, Z. Ouyang and Y. Q. Xia, Biomed. Chromatogr,
2010, 24, 2 –19.
17. I. M.
Valente, L. M. Goncalves and J. A. Rodrigues, J. Chromatogr.
A, 2013, 1308, 58 –62.
18. M.
Gupta, A. Jain and K. K. Verma, J. Sep. Sci., 2010, 33, 3774–3780.
19. Luc Humbert, Michel L hermitte,
in Toxicological Aspects of Drug-Facilitated Crimes,
2014.
20. Allanson, J. P.; Biddlecomebe, R.
A; Jones, A. E.; Pleasance, S. Rapid Coom. Mass Spectrom. .996, 10,811-16.
21. H. Q.
Wu, J. Zhang, K. Norem and T. A. El-Shourbagy, J. Pharm. Biomed. Sci., 2008, 48, 1243–1248. 59
P. L. Kole, G. Venkatesh, J. Kotecha and R. Sheshala, Biomed. Chromatogr,
2011, 25, 199–217. 60 Y. Zhang, H. Cao and H. Jiang, Bioanalysis, 2013, 5, 285–
288.
22. J.
Zhang, H. Q. Wu, E. Kim and T. A. El-Shourbagy,
Biomed. Chromatogram, 2009, 23, 419–425.
23. D. Stevenson, in Encyclopedia of Separation Science,
2000.
24. CAMEL V. Solid phase extraction of trace elements. SpectrochimicaActa B 58, 1177, 2003.
25. Allanson,
J. P., Biddlecombe, R. A., Jones, A. E. and Pleasance, S. 1996. The Use of
Automated Solid Phase Extraction in The ‘96 Well’
Format for High Throughput Bioanalysis Using Liquid Chromatography Coupled to
Tandem Mass Spectrometry. Rapid Communications in Mass Spectrometry 10:811.
26. US
FDA Guidance for Industry, Bioanalytical Method Validation (2015 and
2018).
27. W. Naidong,
W.Z. Shou, T. Addison, S. Maleki, X. Jiang, Rapid Commun. Mass Spectrom. 16 (2002)
1965.
28. X.S. Tong, J. Wang, S.
Zheng, J.V. Pivnichny, J. Pharm. Biomed. Anal. 35
(2004) 867. [21] R. Ruhl, F.J. Schweigert, J. Chromatogr. B 798 (2003) 309
29. Q. Song, H. Junga, Y. Tang, A.C. Li, T. Addison, M. McCort-Tipton,
B. Beato, W. Naidong, J. Chromatogr. B 814 (2005) 105.
30. Y.-J. Xue, J. Liu, J. Pursley, S.
Unger, J. Chromatogr. B 831 (2006) 213. [15]
31. M.C. Rouan, C. Buffet, F. Marfil, H.
Humbert, G. Maurer, J. Pharm. Biomed. Anal. 25 (2001) 995.
32. V. Pucci, E. Monteagudo, F. Bonelli, Rapid Commun. Mass Spectrom. 19 (2005)
3713
33. W.Z. Shou, X. Jiang,
B.D. Beato, W. Naidong,
Rapid Commun. Mass Spectrom.
15 (2001) 466.
34. H. Kim, M.S. Jang,
J.-A. Lee, D. Pyo, H.-R. Yoon, H.J. Lee, K.R. Lee, Chromatographia 60 (2004) 335
35. Larsen,
B. S.; McEwen, C. N. Mass Spectrometry of Biological Materials, 2nd. ed.;
Marcel Dekker: New York, 1998. 81-98.
36. Slobodnik, J. H. et al. / Chromatogr.
A. 1996, 741, 59-74.
37. Katajamaa, M. and Oresic, M. (2005) Processing Methods for Differential
Analysis Of LC/MS Profile Data. BMC Bioinformatics, 6, 179
38. Li,
X. J. et al. (2005) A Software Suite for The Generation and Comparison
of Peptide Arrays from Sets of Data Collected by Liquid Chromatography-Mass
Spectrometry. Mol. Cell Proteomics, 4, 1328–1340.
39. Ma Ji, et al. A
Fully Automated Plasma Protein Precipitation Sample Preparation Method for
LC–MS/MS Bioanalysis, Journal of Chromatography B, 862 (2008) 219–226.
40. Y.-J. Xue, J. Liu, J. Pursley, S.
Unger, J. Chromatogr. B 831 (2006) 213.
41. Domon, B. and Aebersold, R. (2006) Mass Spectrometry and Protein
Analysis. Science, 312, 212–217.
42. Wang, P. et al.
(2006a) A Statistical Method for Chromatographic Alignment of LC-MS Data.
Biostatistics.
43. Honda Akira et al
Highly Sensitive Quantification of Key Regulatory Oxysterols in Biological
Samples by LC-ESI-MS/MS 2015)
44. Zhang, Z., D. Li, D.
E. Blanchard, S. R. Lear, S. K. Erickson, and T. A. Spencer. 2001. Key
Regulatory Oxysterols in Liver: Analysis as D4-3-Ketone Derivatives by HPLC and
Response to Physiological Perturbations. J. Lipid Res
45. Honda, A., K.
Yamashita, H. Miyazaki, M. Shirai, T. Ikegami, G. Xu, M. Numazawa,
T. Hara, and Y. Matsuzaki. Highly Sensitive Analysis
of Sterol Profiles in Human Serum by LC-ESI-MS/MS. J. Lipid Res2008.
46. Masukawa, Y., and H. Tsujimura. 2007. Highly Sensitive Determination of Diverse
Ceramides in Human Hair Using Reversed-Phase Highperformance
Liquid Chromatography-Electrospray Ionization Mass Spectrometry.
47. Farwanah, H., J. Wirtz, T.
Kolter, K. Raith, R. H. Neubert, and K. Sandhoff 2009. Normal Phase Liquid Chromatography Coupled
to Quadrupole Time Of fl Ight Atmospheric
Pressure Chemical Ionization Mass Spectrometry for Separation, Detection and
Mass Spectrometric Profiling of Neutral Sphingolipids and Cholesterol. J.
Chromatogr. B Analyt.
Technol. Biomed. Life Sci. 877: 2976 – 2982.
48. SmedenJeroen van et al.
LC/MS Analysis of Stratum Corneum Lipids: Ceramide Profiling and
Discovery, 2011.
49. Masukawa, Y.,
H. Narita, E. Shimizu, N. Kondo, Y. Sugai, T. Oba, R.
Homma, J. Ishikawa, Y. Takagi, T. Kitahara, et al.
2008. Characterization of overall ceramide species in human stratum corneum. J.
Lipid Res.
50. Motta,
S., M. Monti, S. Sesana, R. Caputo, S. Carelli, and R. Ghidoni. 1993.
Ceramide Composition of the Psoriatic Scale. Biochim.
Biophys. Acta)
51. Zhang Aihua, F. Courant, G. Pinel, E. Bichon, F. Monteau, J. P. Antignac and B. Le Bizec, Analyst, 2009, 134, 1637–1646.
52. J. Chen, X. Zhang, R. Cao, X. Lu, S. Zhao, A. Fekete, Q. Huang, P. Schmitt-Kopplin, Y. Wang, Z. Xu, X. Wan, X. Wu, N. Zhao, C. Xu and G. Xu, J. Proteome Res., 2011, 10, 2625–2632.
53. J. R. Denery, A. A. Nunes, M. S. Hixon, T. J. Dickerson and K. D. Janda, PLoS Neglected Trop. Dis., 2010, 4, e83.
54. S. Bajad and V. Shulaev, Methods Mol. Biol., 2011, 708, 213–228.
55. H. Lv, G. Palacios, K. Hartil and I. J. Kurland, J. Proteome Res., 2011, 10, 2104–2112.
56. Sun Hui, Wang Ping, Han Ying and Wang Xijun, Modern Analytical Techniques in Metabolomics Analysis 2012.
57. Chace, Kalas, and Naylor the Application of Tandem Mass Spectrometry to Neonatal Screening for Inherited Disorders of Intermediary Metabolism First published online as a Review in Advance on May 7, 2002.
58. Carpentera Kevin H., Wiley Veronica, Application of tandem mass spectrometry to biochemical genetics and new born screening Clinica Chimica Acta 322 (2002) 1–10
59. Kushnir Mark M., Rockwood Alan L., and Bergquist Jonas Liquid Chromatography–Tandem Mass Spectrometry Applications in Endocrinology Published online 25 August 2009 in Wiley Inter Science.
60. Hanold KA, Fischer SM, Cormia PH, Miller CE, Syage JA. 2004. Atmospheric pressure photoionization. General properties for LC/ MS. Anal Chem 76:2842–2851.
61. Sannino Anna, Bolzoni Luciana and Bandini Mirella Application of Liquid Chromatography with Electrospray Tandem Mass Spectrometry to The Determination of A New Generation of Pesticides in Processed Fruits and Vegetables Journal of Chromatography A, 1036 (2004) 161–169
62. M.J. Taylor, K. Hunter, K.B. Hunter, D. Lindsay, S. Le Bouhellec, J. Chromatogr. A 982 (2002) 225
63. Detlef Thieme and Hans Sachs Improved Screening Capabilities in Forensic Toxicology By Application of Liquid Chromatography–Tandem Mass Spectrometry Analytica Chimica Acta 492 (2003) 171–186
Received on 20.04.2020 Modified on 31.05.2020
Accepted on 23.06.2020 ©Asian Pharma Press All Right Reserved
Asian J. Pharm. Ana. 2020; 10(3):165-172.
DOI: 10.5958/2231-5675.2020.00030.7