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1.
Anal Chem ; 95(10): 4592-4596, 2023 03 14.
Article in English | MEDLINE | ID: mdl-36802528

ABSTRACT

Liquid chromatography-high-resolution mass spectrometry (LC-HRMS) is widely used to detect chemicals with a broad range of physiochemical properties in complex biological samples. However, the current data analysis strategies are not sufficiently scalable because of data complexity and amplitude. In this article, we report a novel data analysis strategy for HRMS data founded on structured query language database archiving. A database called ScreenDB was populated with parsed untargeted LC-HRMS data after peak deconvolution from forensic drug screening data. The data were acquired using the same analytical method over 8 years. ScreenDB currently holds data from around 40,000 data files, including forensic cases and quality control samples that can be readily sliced and diced across data layers. Long-term monitoring of system performance, retrospective data analysis for new targets, and identification of alternative analytical targets for poorly ionized analytes are examples of ScreenDB applications. These examples demonstrate that ScreenDB makes a significant improvement to forensic services and that the concept has potential for broad applications for all large-scale biomonitoring projects that rely on untargeted LC-HRMS data.


Subject(s)
Forensic Medicine , Retrospective Studies , Mass Spectrometry/methods , Chromatography, Liquid/methods
2.
J Sep Sci ; 36(2): 246-51, 2013 Jan.
Article in English | MEDLINE | ID: mdl-23255186

ABSTRACT

An ultra-performance LC TOF MS method for quantitative analysis of cortisol and 6ß-hydroxycortisol in urine was developed. The method was used for determination of the ratio between 6ß-hydroxycortisol and cortisol in urine received from autopsy cases and living persons as a measure of cytochrome P450 3A enzyme activity. Urine samples (0.25 mL) were extracted with an in-house developed fully automated 96-well SPE system. The compounds were quantified using a Waters ACQUITY UPLC system coupled to a Waters SYNAPT G2. The MS sensitivity was optimized by using negative ionization in sensitivity mode (resolution >10 000 full-width at half-maximum), and further optimized by using the enhanced duty cycle around the 410 m/z. ESCi (simultaneous electrospray and atmospheric pressure chemical ionization) mode was used to compensate for the matrix effects of postmortem urine. Finally, the SYNAPT G2 was tested as a quantitative instrument. The developed method has a measurement range from 2.5-300 ng/mL for cortisol to 10-1200 ng/mL for 6ß-hydroxycortisol. Mean overall process efficiencies were 29.4 and 23.0% for cortisol and 6ß-hydroxycortisol, respectively. In 20 forensic reference cases, the range of the 6ß-hydroxycortisol/cortisol ratio was 0.29-14.2 with a median of 3.04.


Subject(s)
Chromatography, High Pressure Liquid/methods , Hydrocortisone/analogs & derivatives , Hydrocortisone/urine , Solid Phase Extraction/methods , Tandem Mass Spectrometry/methods , Automation , Chromatography, High Pressure Liquid/instrumentation , Humans , Solid Phase Extraction/instrumentation , Spectrometry, Mass, Electrospray Ionization/instrumentation , Spectrometry, Mass, Electrospray Ionization/methods , Tandem Mass Spectrometry/instrumentation
3.
Metabolites ; 2(1): 214-20, 2012 Feb 23.
Article in English | MEDLINE | ID: mdl-24957375

ABSTRACT

Atlantinone A has been isolated from the psychrotolerant fungus Penicillium ribeum. The exact structure of the compound was confirmed by mass spectrometric and 1- and 2D NMR experiments. Atlantinone A was originally only produced upon chemical epigenetic manipulation of P. hirayamae, however in this study the compound was found to be produced at standard growth conditions by the following species; P. solitum, P. discolor, P. commune, P. caseifulvum, P. palitans, P. novae-zeelandiae and P. monticola. A biosynthetic pathway to atlantinone A starting from andrastin A is proposed.

4.
Drug Test Anal ; 4(5): 342-54, 2012 May.
Article in English | MEDLINE | ID: mdl-22102551

ABSTRACT

The ability of forensic laboratories to detect and identify unknown compounds is highly important since new, non-controlled designer drugs are appearing on the market with increasing frequency. In this study, the combined use of gas chromatography-mass spectrometry (GC-MS) and ultra performance liquid chromatography-quadrupole time of flight-mass spectrometry (UPLC-QTOF-MS) was used for screening of new unknowns. In one large seizure from a Danish Internet company, ten different drugs were identified. Several of the compounds were seized for the first time in Denmark. The GC-MS and UPLC-QTOF-MS analyses were supplemented by nuclear magnetic resonance (NMR) spectra for the structural elucidation of p-fluoroamphetamine, mephedrone (4-methylmethcathinone), flephedrone (4-fluoromethcathinone), PPP (α-pyrrolidinopropiophenone), MDPV (3,4-methylenedioxypyrovalerone), Bk-MBDB (2-methylamino-1-(3,4-methylenedioxyphenyl)butan-1-one), pFBT (3-(pfluorobenzoyl)-tropane), and JWH-073 (1-butyl-3-(1-naphthoyl)indol), whereas methylone (3,4-methylenedioxymethcathinone) and N-ethylcathinone matched electron impact-mass spectrometry (EI-MS) library spectra and therefore the screenings were considered sufficient. EI-MS spectra and the proposed main fragmentation patterns are presented as well as QTOF-MS exact masses and fragments and NMR chemical shifts. For the ß-ketophenylethylamines (mephedrone, flephedrone, PPP, MDPV, Bk-MBDB, methylone, and N-ethylcathinone) some general fragmentation patterns observed in the EI-MS and QTOF-MS spectra are further discussed and compared to other ß-ketophenylethylamines.


Subject(s)
Designer Drugs/analysis , Magnetic Resonance Spectroscopy , Mass Spectrometry , Chromatography, High Pressure Liquid , Denmark , Gas Chromatography-Mass Spectrometry
5.
J Agric Food Chem ; 55(18): 7489-94, 2007 Sep 05.
Article in English | MEDLINE | ID: mdl-17696360

ABSTRACT

The composition of noni (Morinda citrifolia) products has been investigated. TLC profiles of several commercial juices and capsules were compared. 3-Methyl-1,3-butanediol was identified as a typical marker in noni juices. The presence of sorbic acid (E200) was detected in one juice declared as additive free. Quantitative data have been obtained by HPLC-MS. A method for the quantification of characteristic noni constituents, such as iridoid glucosides, scopoletin, rutin, fatty acid glucosides, and anthraquinones, was developed and validated. The separation was performed on a C18 column with a gradient of acetonitrile in water containing 0.1% formic acid. Detection was carried out with ESI-MS in the negative ion mode. Significant differences were observed between the products. Asperulosidic acid, deacetylasperulosidic acid, and rutin were present in all samples analyzed, but their concentrations differed considerably between the products. Fatty acid glucosides, noniosides B and C, were present in capsules and most juices. Scopoletin was mainly found in juices. The anthraquinone alizarin, which has been reported from roots and leaves, was not detected in the samples investigated.


Subject(s)
Food Preservation , Fruit/chemistry , Morinda/chemistry , Chromatography, High Pressure Liquid , Mass Spectrometry
6.
Planta Med ; 72(14): 1322-7, 2006 Nov.
Article in English | MEDLINE | ID: mdl-17051459

ABSTRACT

Four new trisaccharide fatty acid esters named noniosides E - H ( 4 - 7) were isolated from the fruit of Morinda citrifolia (Noni) by a combination of Sephadex LH-20, high-speed countercurrent chromatography (HSCCC) and semipreparative HPLC. Their structures were elucidated by high resolution mass spectrometry and 1D- and 2D-NMR as 2,6-di- O-(beta-D-glucopyranosyl)-1-O-hexanoyl-beta-D-glucopyranose (4), 2,6-di-O-(beta-D-glucopyranosyl)-1-O-decanoyl-beta-D-glucopyranose (5), 2-O-(6-O-octanoyl-beta-D-glucopyranosyl)-6-O-(beta-D-glucopyranosyl)-1-O-octanoyl-beta-D-glucopyranose (6), and 2-O-(6-O-hexanoyl-beta-D-glucopyranosyl)-6-O-(beta-D-glucopyranosyl)-1-O-octanoyl-beta-D-glucopyranose or 2-O-(6-O-octanoyl-beta-D-glucopyranosyl)-6-O-(beta-D-glucopyranosyl)-1-O-hexanoyl-beta-D-glucopyranose (7), respectively. In addition, an HPLC-MS analysis of a methanolic extract of the fruit powder revealed the presence of further derivatives including new disaccharide and trisaccharide esters with fatty acid residues of various lengths.


Subject(s)
Glycolipids/chemistry , Morinda , Phytotherapy , Plant Extracts/chemistry , Chromatography, High Pressure Liquid , Esters/chemistry , Fatty Acids/chemistry , Fruit , Humans , Magnetic Resonance Spectroscopy , Mass Spectrometry , Trisaccharides/chemistry
7.
Int J Syst Evol Microbiol ; 56(Pt 6): 1427-1437, 2006 Jun.
Article in English | MEDLINE | ID: mdl-16738124

ABSTRACT

Penicillium jamesonlandense is a novel species from Greenland that grows exceptionally slowly at 25 degrees C and has an optimum temperature for growth of 17-18 degrees C. The novel species is more psychrotolerant than any other Penicillium species described to date. Isolates of this novel species produce a range of secondary metabolites with a high chemical diversity, represented by kojic acid, penicillic acid, griseofulvin, pseurotin, chrysogine, tryptoquivalins and cycloaspeptide. Penicillium ribium, another novel psychrotolerant species from the Rocky Mountains, Wyoming, USA, produces asperfuran, kojic acid and cycloaspeptide. Originally reported from an unidentified Aspergillus species isolated from Nepal, cycloaspeptide A is reported here for the first time from the two novel Penicillium species and two known psychrotolerant species with high chemical diversity, Penicillium soppii and Penicillium lanosum. All species, except P. ribium, produce a combination of cycloaspeptide and griseofulvin. However, P. ribium (3/5 strains) produced the precursor to griseofulvin, norlichexanthone. The type strain of Penicillium jamesonlandense sp. nov. is DAOM 234087(T) (=IBT 21984(T) = IBT 24411(T) = CBS 102888(T)) and the type strain of Penicillium ribium sp. nov. is DAOM 234091(T) (=IBT 16537(T) = IBT 24431(T)).


Subject(s)
Penicillium/classification , Penicillium/genetics , Peptides, Cyclic/genetics , Genetic Variation , Molecular Sequence Data , Penicillium/growth & development , Penicillium/isolation & purification , Phylogeny , Soil Microbiology
8.
Mycol Res ; 109(Pt 11): 1243-9, 2005 Nov.
Article in English | MEDLINE | ID: mdl-16279417

ABSTRACT

A survey of Penicillium albocoremium was undertaken to identify potential taxonomic metabolite markers. One major and four minor metabolites were consistently produced by the 19 strains surveyed on three different media. Following purification and spectral studies, the metabolites were identified as the known protein farnesyl transferase inhibitors andrastin A (1) and barceloneic acid A (2) along with barceloneic acid B (3), barceloneic lactone (4), and methyl barceloneate (5). These compounds are significant taxonomic markers for P. albocoremium; moreover this is the first report of a methyl ester of a barceloneic acid being produced as a secondary metabolite. Tissue extracts created following pathogenicity trials involving P. albocoremium and Allium cepa confirmed the production of these five metabolites in planta. Barceloneic acid B was found to be biologically active against a P388 murine leukemia cell line.


Subject(s)
Alkyl and Aryl Transferases/antagonists & inhibitors , Androstadienes/pharmacology , Enzyme Inhibitors/pharmacology , Onions/microbiology , Penicillium/metabolism , Phenyl Ethers/pharmacology , Salicylates/pharmacology , Alkyl and Aryl Transferases/metabolism , Androstadienes/chemistry , Androstadienes/metabolism , Animals , Cell Line, Tumor , Crystallography, X-Ray , Enzyme Inhibitors/chemistry , Enzyme Inhibitors/metabolism , Inhibitory Concentration 50 , Mice , Nuclear Magnetic Resonance, Biomolecular , Phenyl Ethers/chemistry , Phenyl Ethers/metabolism , Salicylates/chemistry , Salicylates/metabolism , Spectrometry, Mass, Electrospray Ionization
9.
J Antibiot (Tokyo) ; 58(2): 141-4, 2005 Feb.
Article in English | MEDLINE | ID: mdl-15835725

ABSTRACT

A new cyclic nitropeptide, psychrophilin D (1), together with two known cyclic peptides, cycloaspeptide A (2) and cycloaspeptide D (3), were isolated from the psychrotolerant fungus Penicillium algidum using C18 flash chromatography, LH-20 Sephadex and preparative HPLC. The structure of psychrophilin D (1) was derived from mass spectrometric information, 1D and 2D NMR spectra and Marfey's method. The compounds were tested in antimicrobial, antiviral, anticancer and antiplasmodial assays. Psychrophilin D (1) exhibited a moderate activity (ID50 10.1 microg/ml) in the P388 murine leukaemia cell assay. Cycloaspeptide A (2) and D (3) exhibited moderate activity (IC50 3.5 and 4.7 microg/ml, respectively) against Plasmodium falciparum.


Subject(s)
Anti-Bacterial Agents/pharmacology , Penicillium/chemistry , Peptides, Cyclic/pharmacology , Animals , Anti-Bacterial Agents/isolation & purification , Antibiotics, Antineoplastic/pharmacology , Antimalarials/pharmacology , Antiviral Agents/pharmacology , Bacteria/drug effects , Cell Line, Tumor , Chromatography, High Pressure Liquid , Circular Dichroism , Drug Screening Assays, Antitumor , Humans , Leukemia P388/drug therapy , Magnetic Resonance Spectroscopy , Mass Spectrometry , Mice , Microbial Sensitivity Tests , Peptides, Cyclic/isolation & purification , Plasmodium falciparum/drug effects , Viruses/drug effects
10.
J Nat Prod ; 68(2): 258-61, 2005 Feb.
Article in English | MEDLINE | ID: mdl-15730257

ABSTRACT

Communesins G (1) and H (2), two new alkaloids, have been isolated from the psychrotolerant, new species Penicillium rivulum Frisvad. The compounds were isolated by high-speed countercurrent chromatography and preparative HPLC using UV-guided fractionation. The structures were determined from 1D and 2D NMR techniques and HRESIMS. In contrast to all other known communesins, 1 and 2 were found inactive in antimicrobial, antiviral, and anticancer assays.


Subject(s)
Alkaloids/isolation & purification , Heterocyclic Compounds, 4 or More Rings/isolation & purification , Penicillium/chemistry , Alkaloids/chemistry , Alkaloids/pharmacology , Chromatography, High Pressure Liquid , Denmark , Heterocyclic Compounds, 4 or More Rings/chemistry , Heterocyclic Compounds, 4 or More Rings/pharmacology , Molecular Structure , Nuclear Magnetic Resonance, Biomolecular
11.
J Nat Prod ; 67(12): 2111-2, 2004 Dec.
Article in English | MEDLINE | ID: mdl-15620265

ABSTRACT

Karnatakafurans A (1) and B (2), two novel dibenzofurans, have been isolated from the Specie Novum Aspergillus karnatakaensis Frisvad. The compounds were the major secondary metabolites and were isolated through UV-guided fractionation of the organic extract. The structures were elucidated by spectroscopic methods including MS and NMR. The compounds were tested for antimicrobial and antimalarial activity and proved to be moderately active against Plasmodium falciparum.


Subject(s)
Antimalarials/isolation & purification , Aspergillus/chemistry , Plasmodium falciparum/drug effects , Animals , Antimalarials/chemistry , Antimalarials/pharmacology , Benzofurans , Magnetic Resonance Spectroscopy , Mass Spectrometry , Microbial Sensitivity Tests , Molecular Structure
12.
J Nat Prod ; 67(11): 1950-2, 2004 Nov.
Article in English | MEDLINE | ID: mdl-15568799

ABSTRACT

Psychrophilins B (1) and C (2), two new cyclic nitropeptides, have been isolated from the psychrotolerant, new species Penicillium rivulum Frisvad. The nitropeptides were isolated by high-speed countercurrent chromatography (HSCCC) and HPLC using UV-guided fractionation of the organic extract.


Subject(s)
Penicillium/chemistry , Peptides, Cyclic/isolation & purification , Chromatography, High Pressure Liquid , Molecular Conformation , Molecular Structure , Nuclear Magnetic Resonance, Biomolecular , Peptides, Cyclic/chemistry , Peptides, Cyclic/pharmacology
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