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Development of a single-run liquid chromatography-mass spectrometry analysis for the detection of 11 multiclass contaminants of emerging concern using a direct filtration method

Razak MR, Aris AZ, Sukatis FF, Zaki MRM, Zainuddin AH, Haron DEM, et al.

J Sep Sci, 2023 Jan;46(1):e2200282.
PMID: 36337037 DOI: 10.1002/jssc.202200282

In toxicological analysis, the analytical validation method is important to assess the exact risk of contaminants of emerging concern in the environment. Syringe filters are mainly used to remove impurities from sample solutions. However, the loss of analyte to the syringe filter could be considerable, causing an underestimate of the analyte concentrations. The current study develops and validates simultaneous liquid chromatography-mass spectrometry analysis using a direct filtration method to detect four groups of contaminants of emerging concern. The adsorption of the analyte onto three different matrices and six types of syringe filters is reported. The lowest adsorption of analytes was observed in methanol (16.72%), followed by deionized water (48.19%) and filtered surface lake water (48.94%). Irrespective of the type of the matrices, the lowest average adsorption by the syringe filter was observed in the 0.45 μm polypropylene membrane (15.15%), followed by the 0.20 μm polypropylene membrane (16.10%), the 0.20 μm regenerated cellulose (16.15%), the 0.20 μm polytetrafluoroethylene membrane (47.38%), the 0.45 μm nylon membrane (64.87%) and the 0.20 μm nylon membrane (71.30%). In conclusion, the recommended syringe filter membranes for contaminants of emerging concern analysis are polypropylene membranes and regenerated cellulose, regardless of the matrix used.

Matched MeSH terms: Chromatography, Liquid
Fulltext Detection of Pork in Beef Meatballs Using LC-HRMS Based Untargeted Metabolomics and Chemometrics for Halal Authentication

Windarsih A, Riswanto FDO, Bakar NKA, Yuliana ND, Dachriyanus, Rohman A

Molecules, 2022 Nov 29;27(23).
PMID: 36500423 DOI: 10.3390/molecules27238325

Adulteration of high-quality meat products using lower-priced meats, such as pork, is a crucial issue that could harm consumers. The consumption of pork is strictly forbidden in certain religions, such as Islam and Judaism. Therefore, the objective of this research was to develop untargeted metabolomics using liquid chromatography-high resolution mass spectrometry (LC-HRMS) combined with chemometrics for analysis of pork in beef meatballs for halal authentication. We investigated the use of non-targeted LC-HRMS as a method to detect such food adulteration. As a proof of concept using six technical replicates of pooled samples from beef and pork meat, we could show that metabolomics using LC-HRMS could be used for high-throughput screening of metabolites in meatballs made from beef and pork. Chemometrics of principal component analysis (PCA) was successfully used to differentiate beef meatballs and pork meatball samples. Partial least square-discriminant analysis (PLS-DA) clearly discriminated between halal and non-halal beef meatball samples with 100% accuracy. Orthogonal projection to latent structures-discriminant analysis (OPLS-DA) perfectly discriminated and classified meatballs made from beef, pork, and a mixture of beef-pork with a good level of fitness (R2X = 0.88, R2Y = 0.71) and good predictivity (Q2 = 0.55). Partial least square (PLS) and orthogonal PLS (OPLS) were successfully applied to predict the concentration of pork present in beef meatballs with high accuracy (R2 = 0.99) and high precision. Thirty-five potential metabolite markers were identified through VIP (variable important for projections) analysis. Metabolites of 1-(1Z-hexadecenyl)-sn-glycero-3-phosphocholine, acetyl-l-carnitine, dl-carnitine, anserine, hypoxanthine, linoleic acid, and prolylleucine had important roles for predicting pork in beef meatballs through S-line plot analysis. It can be concluded that a combination of untargeted metabolomics using LC-HRMS and chemometrics is promising to be developed as a standard analytical method for halal authentication of highly processed meat products.

Matched MeSH terms: Chromatography, Liquid
Electrokinetic Extraction of Doxorubicin from Biological Fluids by Polymer Inclusion Membrane Sampling Probe

Tey HY, Breadmore MC, See HH

Anal Chem, 2023 Jan 31;95(4):2134-2139.
PMID: 36649064 DOI: 10.1021/acs.analchem.2c02937

A polymer inclusion membrane (PIM) based sampling probe was developed for electrokinetic extraction of drugs from biological fluids. The probe was fabricated by dip-coating a nonconductive glass capillary tube in a homogeneous PIM solution for three cycles. The PIM solution comprised cellulose triacetate (CTA), 2-nitrophenyl octyl ether (NPOE), and 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide [EMIM][NTf2] in a ratio of 5:4:2. The developed probe electrokinetically extracted doxorubicin from human plasma, human serum, and dried blood spot (DBS). The practicability and reliability of the electrokinetic extraction were evaluated by LC-MS/MS to quantify the desorption of extracted doxorubicin. Under the optimized conditions, a quantification limit of 0.2-2 ng/mL was achieved for the three biological samples. The probe was further integrated into a portable battery-powered device for safe low-voltage (36 V) electrokinetic extraction. The developed technique is envisioned to provide a more efficient analytical workflow in the laboratory.

Matched MeSH terms: Chromatography, Liquid
Effects of high-voltage electrostatic field (HVEF) on frozen shrimp (Solenocera melantho) based on UPLC-MS untargeted metabolism

Liu J, Zhu F, Yang J, Wang Y, Ma X, Lou Y, et al.

Food Chem, 2023 Jun 15;411:135499.
PMID: 36696717 DOI: 10.1016/j.foodchem.2023.135499

Shrimp meat is prone to autolysis and decay due to the abundance of endogenous enzymes and contamination from microorganisms. HVEF freezing can slow the spoilage of shrimp, producing small and uniform ice crystals, resulting in less damage to muscle tissue. In this study, HVEF technique was used to freeze the shrimp (Solenocera melantho), and the UPLC-MS metabolic technique was used to investigate the metabolites of frozen shrimp meat. Compared with the control group, 367 differential metabolites were identified in the HVEF group. Mapping them to the KEGG database, there were 108 with KEGG ID. Purine metabolism and pyrimidine metabolism were the most enriched pathways. In addition, phosphatidylcholines (PCs), inosine (HxR), and l-valine were identified as potential biomarkers associated with lipid, nucleotide, and organic acid metabolism, respectively. Overall, HVEF can improve freezing quality of shrimp meat by slowing down the metabolism of substances in the muscle of S. melantho.

Matched MeSH terms: Chromatography, Liquid
Decomplexation proteomic analysis and purity assessment of a biologic for snakebite envenoming: Philippine Cobra Antivenom

Palasuberniam P, Tan KY, Chan YW, Blanco FB, Tan CH

Trans R Soc Trop Med Hyg, 2023 Jun 02;117(6):428-434.
PMID: 36611268 DOI: 10.1093/trstmh/trac125

BACKGROUND: Philippine Cobra Antivenom (PCAV) is the only snake antivenom manufactured in the Philippines. It is used clinically to treat envenoming caused by the Philippine Spitting Cobra (Naja philippinensis). While PCAV is effective pharmacologically, it is crucial to ensure the safety profile of this biologic that is derived from animal plasma.
METHODS: This study examined the composition purity of PCAV through a decomplexation proteomic approach, applying size-exclusion chromatography (SEC), sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) and tandem mass spectrometry liquid chromatography-tandem mass spectrometry (LC-MS/MS).
RESULTS: SDS-PAGE and SEC showed that the major protein in PCAV (constituting ∼80% of total proteins) is approximately 110 kDa, consistent with the F(ab')2 molecule. This protein is reducible into two subunits suggestive of the light and heavy chains of immunoglobulin G. LC-MS/MS further identified the proteins as equine immunoglobulins, representing the key therapeutic ingredient of this biologic product. However, protein impurities, including fibrinogens, alpha-2-macroglobulins, albumin, transferrin, fibronectin and plasminogen, were detected at ∼20% of the total antivenom proteins, unveiling a concern for hypersensitivity reactions.
CONCLUSIONS: Together, the findings show that PCAV contains a favorable content of F(ab')2 for neutralization, while the antibody purification process awaits improvement to minimize the presence of protein impurities.

Matched MeSH terms: Chromatography, Liquid
Fulltext Pathogenicity of monokaryotic and dikaryotic mycelia of Ganoderma boninense revealed via LC-MS-based metabolomics

Santiago KAA, Wong WC, Goh YK, Tey SH, Ting ASY

Sci Rep, 2024 Mar 04;14(1):5330.
PMID: 38438519 DOI: 10.1038/s41598-024-56129-8

This study compared the pathogenicity of monokaryotic (monokaryon) and dikaryotic (dikaryon) mycelia of the oil palm pathogen Ganoderma boninense via metabolomics approach. Ethyl acetate crude extracts of monokaryon and dikaryon were analysed by liquid chromatography quadrupole/time-of-flight-mass spectrometry (LC-Q/TOF-MS) coupled with multivariate data analysis using MetaboAnalyst. The mummichog algorithm was also used to identify the functional activities of monokaryon and dikaryon without a priori identification of all their secondary metabolites. Results revealed that monokaryon produced lesser fungal metabolites than dikaryon, suggesting that monokaryon had a lower possibility of inducing plant infection. These findings were further supported by the identified functional activities. Monokaryon exhibits tyrosine, phenylalanine, and tryptophan metabolism, which are important for fungal growth and development and to produce toxin precursors. In contrast, dikaryon exhibits the metabolism of cysteine and methionine, arginine and proline, and phenylalanine, which are important for fungal growth, development, virulence, and pathogenicity. As such, monokaryon is rendered non-pathogenic as it produces growth metabolites and toxin precursors, whereas dikaryon is pathogenic as it produces metabolites that are involved in fungal growth and pathogenicity. The LC-MS-based metabolomics approach contributes significantly to our understanding of the pathogenesis of Ganoderma boninense, which is essential for disease management in oil palm plantations.

Matched MeSH terms: Chromatography, Liquid
LC-MS-MS method for mitragynine and 7-hydroxymitragynine in hair and its application in authentic hair samples of suspected kratom abusers

Rhee J, Shin I, Kim J, Lee J, Cho B, Kim J, et al.

J Anal Toxicol, 2024 Jul 13;48(6):429-438.
PMID: 38780234 DOI: 10.1093/jat/bkae041

Kratom is a natural psychoactive product known primarily in Southeast Asia, including Thailand, Malaysia, etc. It is also known as krathom, kakuam, ithang, thom (Thailand), biak-biak, ketum (Malaysia) and mambog (Philippines) and is sometimes used as an opium substitute. It is stimulant at doses of 1-5 g, analgesic at doses of 5-15 g and euphoric and sedative at doses of >15 g. Mitragynine is the most abundant indole compound in kratom (Mitragyna speciosa) and is metabolized in humans to 7-hydroxymitragynine, the more active metabolite. Adverse effects include seizures, nausea, vomiting, diarrhea, tachycardia, restlessness, tremors, hallucinations and death. There are few studies on the analytical method for the detection of mitragynine and 7-hydroxymitragynine in hair. Therefore, this study proposes a liquid chromatography-tandem mass spectrometry (LC-MS-MS) method for the analysis of kratom in hair. Hair samples were first weighed to ∼10 mg and washed with methanol. Then the washed hair samples were cut into pieces and incubated in methanol with stirring and heating (16 h/38℃). Extracts were then analyzed by LC-MS-MS. This method was validated by determining the limit of detection (LOD), limit of quantification, linearity, intra- and inter-day accuracy and precision, recovery and matrix effects. The intra- and inter-day precision (CV%) and accuracy (bias%) were within ±20%, which was considered acceptable. Using this newly developed LC-MS-MS method, the simultaneous detection of mitragynine and 7-hydroxymitragynine in six authentic hair samples was achieved to provide the direct evidence of kratom use in the past. Mitragynine concentrations ranged from 16.0 to 2,067 pg/mg (mean 905.3 pg/mg), and 7-hydroxymitragynine concentrations ranged from 0.34 to 15 pg/mg (mean 7.4 pg/mg) in six authentic hair samples from kratom abusers. This may be due to the higher sensitivity of the LOD in this study, with values of 0.05 pg/mg for mitragynine and 0.2 pg/mg for 7-hydroxymitragynine in hair.

Matched MeSH terms: Chromatography, Liquid
Fulltext Untargeted metabolomics study of mature human milk from women with and without gestational diabetes mellitus

Yao D, Shen C, Zhang X, Tang J, Yu J, Tu M, et al.

Food Chem, 2024 Dec 01;460(Pt 3):140663.
PMID: 39142199 DOI: 10.1016/j.foodchem.2024.140663

Gestational diabetes mellitus (GDM) is a prevalent metabolic disorder during pregnancy that alters the metabolites in human milk. Integrated Gas Chromatography-Mass Spectrometry (GC-MS) and Liquid Chromatography-Mass Spectrometry (LC-MS) were employed for comprehensive identification and comparison of metabolites in mature human milk (MHM) from women with and without GDM. A total of 268 differentially expressed metabolites (DEMs) were identified. Among these, linoleic acid, arachidonic acid, 9R-HODE and L-glutamic acid were significantly elevated and 12,13-DHOME was significantly decreased in MHM of women with GDM. These metabolites are significantly enriched in linoleic acid metabolism, fatty acid biosynthesis, galactose metabolism and ABC transporters pathways. Disorders in these metabolic pathways are associated with insulin resistance and poor glucose metabolism indicating these conditions may persist postpartum.

Matched MeSH terms: Chromatography, Liquid
Chromatographic comparison of atenolol separation in reaction media on cellulose tris-(3,5-dimethylphenylcarbamate) chiral stationary phase using ultra fast liquid chromatography

Agustian J, Kamaruddin AH, Aboul-Enein HY

Chirality, 2012 May;24(5):356-67.
PMID: 22517322 DOI: 10.1002/chir.22019

Because chiral liquid chromatography (LC) could become a powerful tool to estimate racemic atenolol quantity, excellent enantiomeric separation should be produced during data acquisition for satisfactory observation of atenolol concentrations throughout the racemic resolution processes. Selection of chiral LC column and analytical protocol that fulfill demands of the ultra fast LC analysis is essential. This article describes the characteristics of atenolol chromatographic separation that resulted from different resolution media and analytical protocols with the use of a Chiralcel® OD column. The chromatograms showed quite different characteristics of the separation process. The single enantiomer and racemic atenolol could be recognized by the Chiralcel® OD column in less than 20 min. Symmetrical peaks were obtained; however, several protocols produced peaks with wide bases and slanted baselines. Observations showed that efficient enantioresolution of racemic atenolol was obtained at slow mobile phase flow rate, decreased concentration of amine-type modifier but increased alcohol content in mobile phase and highest ultraviolet detection wavelength were required. The optimal ultra fast LC protocol enables to reduce and eliminate the peaks of either the atenolol solvent or the buffers and provided the highest peak intensities of both atenolol enantiomers.

Matched MeSH terms: Chromatography, Liquid/instrumentation; Chromatography, Liquid/methods*
Determination of partition coefficient and analysis of nitrophenols by three-phase liquid-phase microextraction coupled with capillary electrophoresis

Sanagi MM, Miskam M, Wan Ibrahim WA, Hermawan D, Aboul-Enein HY

J Sep Sci, 2010 Jul;33(14):2131-9.
PMID: 20549667 DOI: 10.1002/jssc.201000172

A three-phase hollow fiber liquid-phase microextraction method coupled with CE was developed and used for the determination of partition coefficients and analysis of selected nitrophenols in water samples. The selected nitrophenols were extracted from 14 mL of aqueous solution (donor solution) with the pH adjusted to pH 3 into an organic phase (1-octanol) immobilized in the pores of the hollow fiber and finally backextracted into 40.0 microL of the acceptor phase (NaOH) at pH 12.0 located inside the lumen of the hollow fiber. The extractions were carried out under the following optimum conditions: donor solution, 0.05 M H(3)PO(4), pH 3.0; organic solvent, 1-octanol; acceptor solution, 40 microL of 0.1 M NaOH, pH 12.0; agitation rate, 1050 rpm; extraction time, 15 min. Under optimized conditions, the calibration curves for the analytes were linear in the range of 0.05-0.30 mg/L with r(2)>0.9900 and LODs were in the range of 0.01-0.04 mg/L with RSDs of 1.25-2.32%. Excellent enrichment factors of up to 398-folds were obtained. It was found that the partition coefficient (K(a/d)) values were high for 2-nitrophenol, 3-nitrophenol, 4-nitrophenol, 2,4-dinitrophenol and 2,6-dinitrophenol and that the individual partition coefficients (K(org/d) and K(a/org)) promoted efficient simultaneous extraction from the donor through the organic phase and further into the acceptor phase. The developed method was successfully applied for the analysis of water samples.

Matched MeSH terms: Chromatography, Liquid/instrumentation; Chromatography, Liquid/methods*
Development and validation of a comprehensive solid-phase extraction method followed by LC-TOF/MS for the analysis of eighteen pharmaceuticals in influent and effluent of sewage treatment plants

Al-Qaim FF, Mussa ZH, Yuzir A

Anal Bioanal Chem, 2018 Aug;410(20):4829-4846.
PMID: 29806068 DOI: 10.1007/s00216-018-1120-9

The scarcity of data about the occurrence of pharmaceuticals in water bodies in Malaysia prompted us to develop a suitable analytical method to address this issue. We therefore developed a method based on solid-phase extraction combined with liquid chromatography-time of flight/mass spectrometry (SPE-LC-TOF/MS) for the analysis of sixteen prescribed and two nonprescribed pharmaceuticals that are potentially present in water samples. The levels of these pharmaceuticals, which were among the top 50 pharmaceuticals consumed in Malaysia during the period 2011-2014, in influent and effluent of five sewage treatment plants (STPs) in Bangi, Malaysia, were then analyzed using the developed method. All of the pharmaceuticals were separated chromatographically using a 5 μm, 2.1 mm × 250 mm C18 column at a flow rate of 0.3 mL/min. Limits of quantification (LOQs) were 0.3-8.2 ng/L, 6.5-89 ng/L, and 11.1-93.8 ng/L in deionized water (DIW), STP effluent, and STP influent, respectively, for most of the pharmaceuticals. Recoveries were 51-108%, 52-118%, and 80-107% from the STP influent, STP effluent, and DIW, respectively, for most of the pharmaceuticals. The matrix effect was also evaluated. The signals from carbamazepine, diclofenac sodium, and mefenamic acid were found to be completely suppressed in the STP influent. The signals from other compounds were found to be influenced by matrix effects more strongly in STP influent (enhancement or suppression of signal ≤180%) than in effluent (≤94%). The signal from prednisolone was greatly enhanced in the STP influent, indicating a matrix effect of -134%. Twelve pharmaceuticals were frequently detected in all five STPs, and caffeine, prazosin, and theophylline presented the highest concentrations among all the pharmaceuticals monitored: up to 7611, 550, and 319 ng/L in the STP influent, respectively. To the best of our knowledge, this is the first time that prazosin has been detected in a water matrix in Malaysia. Graphical abstract ᅟ.

Matched MeSH terms: Chromatography, Liquid/instrumentation; Chromatography, Liquid/methods*
A new and simple solid-phase extraction method for LC determination of pyronaridine in human plasma

Ramanathan S, Karupiah S, Nair NK, Olliaro PL, Navaratnam V, Wernsdorfer WH, et al.

J Chromatogr B Analyt Technol Biomed Life Sci, 2005 Sep 25;824(1-2):45-50.
PMID: 16046285

A new approach using a simple solid-phase extraction technique has been developed for the determination of pyronaridine (PND), an antimalarial drug, in human plasma. After extraction with C18 solid-phase sorbent, PND was analyzed using a reverse phase chromatographic method with fluorescence detection (at lambda(ex)=267 nm and lambda(em)=443 nm). The mean extraction recovery for PND was 95.2%. The coefficient of variation for intra-assay precision, inter-assay precision and accuracy was less than 10%. The quantification limit with fluorescence detection was 0.010 microg/mL plasma. The method described herein has several advantages over other published methods since it is easy to perform and rapid. It also permits reducing both, solvent use and sample preparation time. The method has been used successfully to assay plasma samples from clinical pharmacokinetic studies.

Matched MeSH terms: Chromatography, Liquid/instrumentation; Chromatography, Liquid/methods*
Fulltext Wound healing potential of Spirulina platensis extracts on human dermal fibroblast cells

Syarina PN, Karthivashan G, Abas F, Arulselvan P, Fakurazi S

EXCLI J, 2015;14:385-93.
PMID: 27004048 DOI: 10.17179/excli2014-697

Blue-green alga (Spirulina platensis) is a well renowned nutri-supplement due to its high nutritional and medicinal properties. The aim of this study was to examine the wound healing efficiency of Spirulina platensis at various solvent extracts using in vitro scratch assay on human dermal fibroblast cells (HDF). Various gradient solvent extracts (50 μg/ml of methanolic, ethanolic and aqueous extracts) from Spirulina platensis were treated on HDF cells to acquire its wound healing properties through scratch assay and in this investigation we have used allantoin, as a positive control to compare efficacy among the phytoextracts. Interestingly, aqueous extract were found to stimulate proliferation and migration of HDF cells at given concentrations and enhanced closure rate of wound area within 24 hours after treatment. Methanolic and ethanolic extracts have shown proliferative effect, however these extracts did not aid in the migration and closure of wound area when compared to aqueous extract. Based on phytochemical profile of the plant extracts analyzed by LC-MS/MS, it was shown that compounds supposedly involved in accelerating wound healing are cinnamic acid, narigenin, kaempferol, temsirolimus, phosphatidylserine isomeric derivatives and sulphoquinovosyl diacylglycerol. Our findings concluded that blue-green algae may pose potential biomedical application to treat various chronic wounds especially in diabetes mellitus patients.

Matched MeSH terms: Chromatography, Liquid
Recent developments and applications of liquid phase microextraction in fruits and vegetables analysis

Abdulra'uf LB, Sirhan AY, Huat Tan G

J Sep Sci, 2012 Dec;35(24):3540-53.
PMID: 23225719 DOI: 10.1002/jssc.201200427

The sample preparation step has been identified as the bottleneck of analytical methodology in chemical analysis. Therefore, there is need for the development of cost-effective, easy to operate, and environmentally friendly miniaturized sample preparation technique. The microextraction techniques combine extraction, isolation, concentration, and introduction of analytes into analytical instrument, to a single and uninterrupted step, and improve sample throughput. The use of liquid-phase microextraction techniques for the analysis of pesticide residues in fruits and vegetables are discussed with the focus on the methodologies employed by different researchers and their analytical performances. Analytes are extracted using water-immiscible solvents and are desorbed into gas chromatography, liquid chromatography, or capillary electrophoresis for identification and quantitation.

Matched MeSH terms: Chromatography, Liquid
Fulltext Complete genome sequencing of Pandoraea pnomenusa RB38 and Molecular Characterization of Its N-acyl homoserine lactone synthase gene ppnI

Lim YL, Ee R, How KY, Lee SK, Yong D, Tee KK, et al.

PeerJ, 2015;3:e1225.
PMID: 26336650 DOI: 10.7717/peerj.1225

In this study, we sequenced the genome of Pandoraea pnomenusa RB38 using Pacific Biosciences RSII (PacBio) Single Molecule Real Time (SMRT) sequencing technology. A pair of cognate luxI/R homologs was identified where the luxI homolog, ppnI, was found adjacent to a luxR homolog, ppnR1. An additional orphan luxR homolog, ppnR2, was also discovered. Multiple sequence alignment and phylogenetic analysis revealed that ppnI is an N-acyl homoserine lactone (AHL) synthase gene that is distinct from those of the nearest phylogenetic neighbor viz. Burkholderia spp. High resolution tandem mass spectrometry (LC-MS/MS) analysis showed that Escherichia coli BL21 harboring ppnI produced a similar AHL profile (N-octanoylhomoserine lactone, C8-HSL) as P. pnomenusa RB38, the wild-type donor strain, confirming that PpnI directed the synthesis of AHL in P. pnomenusa RB38. To our knowledge, this is the first documentation of the luxI/R homologs of the genus Pandoraea.

Matched MeSH terms: Chromatography, Liquid
Fulltext LC-MS data for metabolomics analysis of Garcinia mangostana L. seed germination

Mazlan O, Aizat WM, Aziz Zuddin NS, Baharum SN, Noor NM

Data Brief, 2018 Dec;21:2221-2223.
PMID: 30555858 DOI: 10.1016/j.dib.2018.11.072

Metabolic regulation is important during seed germination for the establishment of seedling. The germination strategy of mangosteen (Garcinia mangostana L.) seed is thought to be unique due to its recalcitrant characteristic (sensitive to coldness and drying). To investigate the metabolic changes during seed germination, we performed metabolomics analysis on germinating mangosteen seed sown after zero, one, three, five, seven and nine days. Sampled mangosteen seeds were subjected to methanol extraction prior analysis using Liquid Chromatography-Time of Flight-Mass Spectrometry (LC-TOF-MS). MS data were further analyzed using ProfileAnalysis (version 2.1). This is one of the earliest reports in metabolite identification and profiling of mangosteen seed at different germination stages. This data article refers to the article entitled "Metabolite profiling of mangosteen seed germination highlights metabolic changes related to carbon utilization and seed protection" (Mazlan et al., 2019) [1].

Matched MeSH terms: Chromatography, Liquid
Dataset on LC-Q-TOF/MS tentative identification of phytochemicals in the extract of Vernonia amygdalina leaf through positive ionization

Alara OR, Abdurahman NH, Ukaegbu CI, Hassan Z, Kabbashi NA

Data Brief, 2018 Dec;21:1686-1689.
PMID: 30505901 DOI: 10.1016/j.dib.2018.10.159

The tentative identification of bioactive compounds in the extract of Vernonia amygdalina leaf was carried out using positive ionization of Liquid chromatography-mass spectrometry quadrupole time of flight (LC-Q-TOF/MS). The positive ionization is associated with the presence of saponins, flavonoids, alkaloids, terpenoids, and glycosides. Tentative assignments of the secondary metabolites were performed by comparing the MS fragmentation patterns with Waters® UNIFY library which allows positive identification of the compounds based on the spectral match. All the metabolites compounds were estimated and presented in a BPI (Base peak intensity) plot. These data are the unpublished supplementary materials related to "Ethanolic extraction of bioactive compounds from V. amygdalina leaf using response surface methodology as an optimization tool" (Alara et al., 2018).

Matched MeSH terms: Chromatography, Liquid
Fulltext Chemical profile of Xanthine Oxidase inhibitor fraction of Persicaria Hydropiper

Noor Hashim, N.H., Maulidiani, M., Mediani, A., Abas, F.

International Food Research Journal, 2018;25(3):1088-1094.
MyJurnal

Persicaria hydropiper, locally known as kesum, is an herb belongs to the family Polygonaceae. It has been used widely in many countries as food flavoring and possesses a wide range of medicinal values. The total phenolic content and xanthine oxidase inhibitory activity of the methanolic extract of P. hydropiper and fractions were determined spectrophotometrically. The butanol fraction was found to contain high phenolic content and was able to inhibit xanthine oxidase activity. Online profiling using liquid chromatography coupled with electrospray ionisation spectrometry (LC-ESIMS/MS) has revealed ten constituents in this active fraction. The major components were flavonoid derivatives and flavonoid sulphates, which were confirmed by comparison with an authentic standards as well as their MS/MS fragmentation patterns and UV spectra.

Matched MeSH terms: Chromatography, Liquid
Fulltext Data on the optimisation and validation of a liquid chromatography-high-resolution mass spectrometry (LC-HRMS) to establish the presence of phosphodiesterase 5 (PDE5) inhibitors in instant coffee premixes

Mohd Yusop AY, Xiao L, Fu S

Data Brief, 2019 Aug;25:104234.
PMID: 31384643 DOI: 10.1016/j.dib.2019.104234

This paper presents the data on the optimisation and validation of a liquid chromatography-high-resolution mass spectrometry (LC-HRMS) to establish the presence of phosphodiesterase 5 (PDE5) inhibitors and their analogues as adulterants in instant coffee premixes. The method development data covered chromatographic optimisation for better analyte separation and isomeric resolution, mass spectrometry optimisation for high sensitivity and sample preparation optimisation for high extraction recovery (RE) and low matrix effect (ME). The validation data covered specificity, linearity, range, accuracy, limit of detection, limit of quantification, precisions, ME, and RE. The optimisation and validation data presented here is related to the article: "Determination of phosphodiesterase 5 (PDE5) inhibitors in instant coffee premixes using liquid chromatography-high-resolution mass spectrometry (LC-HRMS)" Mohd Yusop et al., 2019.

Matched MeSH terms: Chromatography, Liquid
Fulltext Proteomic Analysis of the Human Anterior Pituitary Gland

Yelamanchi SD, Tyagi A, Mohanty V, Dutta P, Korbonits M, Chavan S, et al.

OMICS, 2018 12;22(12):759-769.
PMID: 30571610 DOI: 10.1089/omi.2018.0160

The pituitary function is regulated by a complex system involving the hypothalamus and biological networks within the pituitary. Although the hormones secreted from the pituitary have been well studied, comprehensive analyses of the pituitary proteome are limited. Pituitary proteomics is a field of postgenomic research that is crucial to understand human health and pituitary diseases. In this context, we report here a systematic proteomic profiling of human anterior pituitary gland (adenohypophysis) using high-resolution Fourier transform mass spectrometry. A total of 2164 proteins were identified in this study, of which 105 proteins were identified for the first time compared with high-throughput proteomic-based studies from human pituitary glands. In addition, we identified 480 proteins with secretory potential and 187 N-terminally acetylated proteins. These are the first region-specific data that could serve as a vital resource for further investigations on the physiological role of the human anterior pituitary glands and the proteins secreted by them. We anticipate that the identification of previously unknown proteins in the present study will accelerate biomedical research to decipher their role in functioning of the human anterior pituitary gland and associated human diseases.

Matched MeSH terms: Chromatography, Liquid

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