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A simple desalting procedure for fast atom bombardment mass spectrometry. 快速原子轰击质谱法的简单脱盐程序。
Biomedical & environmental mass spectrometry Pub Date : 1988-09-01 DOI: 10.1002/bms.1200170312
D C Moon, J A Kelley
{"title":"A simple desalting procedure for fast atom bombardment mass spectrometry.","authors":"D C Moon,&nbsp;J A Kelley","doi":"10.1002/bms.1200170312","DOIUrl":"https://doi.org/10.1002/bms.1200170312","url":null,"abstract":"<p><p>A simple and efficient procedure for desalting samples prior to fast atom bombardment mass spectrometry utilizes low-pressure reverse-phase chromatography with disposable high-capacity mini-columns. Microscale (0.1-10 mumol) sample purification with high analyte recovery is possible for nucleosides, nucleotides and peptides. Salt removal has been evaluated both by conductivity and mass spectral methods and is greater than 99% for the model compounds cytidine, adenosine and AMP, even when they are contaminated with a 10 molar excess of NaCl. This procedure is also applicable to a range of small peptides as demonstrated with pyro-Glu-His-Gly and methionine enkephalin.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170312","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14345579","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 32
Quantification of leukotriene B4 in synovial fluid by gas chromatography/tandem mass spectrometry. 气相色谱/串联质谱法测定滑液中白三烯B4。
Biomedical & environmental mass spectrometry Pub Date : 1988-09-01 DOI: 10.1002/bms.1200170309
M Dawson, C M McGee, P M Brooks, J H Vine, T R Watson
{"title":"Quantification of leukotriene B4 in synovial fluid by gas chromatography/tandem mass spectrometry.","authors":"M Dawson,&nbsp;C M McGee,&nbsp;P M Brooks,&nbsp;J H Vine,&nbsp;T R Watson","doi":"10.1002/bms.1200170309","DOIUrl":"https://doi.org/10.1002/bms.1200170309","url":null,"abstract":"<p><p>A procedure for the quantification of leukotriene B4 (LTB4) in synovial fluid has been developed using gas chromatography/tandem mass spectrometry based on selected reaction monitoring of the elimination of t-butyldimethylsilanol from the ions of m/z 431 and 438 in the negative ion chemical ionization mass spectra of the di-t-butyldimethylsilyl/pentafluorobenzyl derivatives of leukotriene B4 and the internal standard (2H8)leukotriene B4. The detection limit (approximately 10 pg ml-1) is sufficiently low to permit determination of LTB4 concentration in the synovial fluid of patients with various arthropathies. Single-stage mass spectrometry was found not to be selective enough to permit quantification of LTB4 in synovial fluid.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170309","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"13987205","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 88
Evaluation of a high-resolution gas chromatography/high-resolution mass spectrometry method for the determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin in soil and water. 高分辨率气相色谱/高分辨率质谱法测定土壤和水中2,3,7,8-四氯二苯并-对二恶英的评价
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170108
J S Stanley, T M Sack, Y Tondeur, W F Beckert
{"title":"Evaluation of a high-resolution gas chromatography/high-resolution mass spectrometry method for the determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin in soil and water.","authors":"J S Stanley,&nbsp;T M Sack,&nbsp;Y Tondeur,&nbsp;W F Beckert","doi":"10.1002/bms.1200170108","DOIUrl":"https://doi.org/10.1002/bms.1200170108","url":null,"abstract":"<p><p>An analytical protocol for the determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) and total TCDDs in soil, sediment, and aqueous samples using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS) was evaluated through replicate analyses of fortified and unspiked soil and aqueous samples. The results of these analyses demonstrated that the method is useful for the determination of 2,3,7,8-TCDD and total TCDDs at concentrations ranging from 10 to 200 pg/g (ppt) in soil samples and from 100 to 2000 pg/l (ppq) in aqueous samples. Absolute recoveries of the method internal standard, (13C12-2,3,7,8-TCDD, ranged from 24 to 88%. Lower levels of detection can be achieved through a slight modification of the method with respect to initial sample size and/or final extract volume. Instrumental parameters that affect data quality, specifically HRGC column performance, mass resolution and mass measurement accuracy are presented.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170108","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333456","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 8
Identification of the phyto-oestrogen 3',7-dihydroxyisoflavan, an isomer of equol, in human urine and cow's milk. 人尿和牛奶中雌马酚异构体3′，7-二羟基异黄酮的鉴定。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170104
C Bannwart, H Adlercreutz, K Wähälä, T Kotiaho, A Hesso, G Brunow, T Hase
{"title":"Identification of the phyto-oestrogen 3',7-dihydroxyisoflavan, an isomer of equol, in human urine and cow's milk.","authors":"C Bannwart,&nbsp;H Adlercreutz,&nbsp;K Wähälä,&nbsp;T Kotiaho,&nbsp;A Hesso,&nbsp;G Brunow,&nbsp;T Hase","doi":"10.1002/bms.1200170104","DOIUrl":"https://doi.org/10.1002/bms.1200170104","url":null,"abstract":"<p><p>The isoflavonoid diphenol 3',7-dihydroxyisoflavan, an isomer of the known compound equol (4',7-dihydroxyisoflavan), has been identified in human urine and in cow's milk. The compound was isolated as the glucuronide, purified by column chromatography and identified after hydrolysis to the aglycon. The trimethylsilyl ether derivative was characterized by comparison of its mass spectrum and chromatographic properties with those of synthesized silylated isomers of equol.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170104","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333626","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 53
Fast atom bombardment mass spectrometry of some anthracycline and bisanthracycline derivatives. 一些蒽环类和双蒽环类衍生物的快速原子轰击质谱分析。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170107
C J Chandler, R T Brownlee, R J Hook, D R Phillips, J A Reiss, J A Edgar
{"title":"Fast atom bombardment mass spectrometry of some anthracycline and bisanthracycline derivatives.","authors":"C J Chandler,&nbsp;R T Brownlee,&nbsp;R J Hook,&nbsp;D R Phillips,&nbsp;J A Reiss,&nbsp;J A Edgar","doi":"10.1002/bms.1200170107","DOIUrl":"https://doi.org/10.1002/bms.1200170107","url":null,"abstract":"<p><p>Fast atom bombardment (FAB) mass spectra of daunomycin, four of its derivatives, seven bisanthracyclines and three mixed-functional daunomycin-acridine derivatives are reported. These anthracyclines all exhibited their expected [MH]+ ions and peaks corresponding to the fragmentations which are characteristic of the anthracycline moiety, and in addition the spectra showed enhanced [MH + n]+ (n = 1-4) ions which were attributed to reductive processes occurring in the liquid matrix under FAB conditions. Daunomycin was also observed to form a dimeric cluster ion [M2H]+ together with associated reduced ions under FAB conditions. We have found that FAB mass spectrometry is an ideal method for the qualitative analysis of large, non-volatile derivatives of anthracyclines.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170107","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333628","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 3
Separation and identification of trifluralin metabolites by open-tubular liquid chromatography/negative chemical ionization mass spectrometry. 开管液相色谱/负化学电离质谱法分离鉴定曲霉灵代谢物。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170110
J S de Wit, C E Parker, K B Tomer, J W Jorgenson
{"title":"Separation and identification of trifluralin metabolites by open-tubular liquid chromatography/negative chemical ionization mass spectrometry.","authors":"J S de Wit,&nbsp;C E Parker,&nbsp;K B Tomer,&nbsp;J W Jorgenson","doi":"10.1002/bms.1200170110","DOIUrl":"https://doi.org/10.1002/bms.1200170110","url":null,"abstract":"<p><p>The utility of combined open-tubular liquid chromatography/negative ion chemical ionization (NCI) mass spectrometry for the separation and analysis of trifluralin, a commonly used pre-emergence herbicide, and seven of its metabolites has been demonstrated. The NCI mass spectra for these compounds are reported. Some of the NCI mass spectra were obtained from as little as 50 pg of analyte.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170110","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333458","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 13
Practical hints for peptide sequencing by soft ionization methods. 软电离法肽测序的实用提示。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170106
W Kausler, K Schneider, G Spiteller
{"title":"Practical hints for peptide sequencing by soft ionization methods.","authors":"W Kausler,&nbsp;K Schneider,&nbsp;G Spiteller","doi":"10.1002/bms.1200170106","DOIUrl":"https://doi.org/10.1002/bms.1200170106","url":null,"abstract":"<p><p>Practical hints are summarized for the investigation of peptides by soft ionization methods based on liquid secondary ion mass spectrometry. The method aims: to purify the sample; to force a peptide to the surface by ion pair formation; to recover the sample used for mass spectral analysis; to distinguish between Lys and Gln by derivatization; to spot amino acids in the low mass region; and to improve sequence information by use of peptide fragments, not described previously.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170106","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333627","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 16
Relationship of molecular radical anion abundance and calculated lowest unoccupied molecular orbital energies for polychlorinated dibenzofurans and dibenzodioxins in electron capture negative ion mass spectrometry: evidence for negative metastable ions. 电子俘获负离子质谱法中多氯二苯并呋喃和二苯并二恶英分子自由基阴离子丰度与计算的最低未占据分子轨道能的关系:负亚稳离子存在的证据。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170112
J A Laramée, Y S Chang, B C Arbogast, M L Deinzer
{"title":"Relationship of molecular radical anion abundance and calculated lowest unoccupied molecular orbital energies for polychlorinated dibenzofurans and dibenzodioxins in electron capture negative ion mass spectrometry: evidence for negative metastable ions.","authors":"J A Laramée,&nbsp;Y S Chang,&nbsp;B C Arbogast,&nbsp;M L Deinzer","doi":"10.1002/bms.1200170112","DOIUrl":"https://doi.org/10.1002/bms.1200170112","url":null,"abstract":"<p><p>Relationships were found between experimentally measured molecular radical anion abundances and calculated lowest unoccupied molecular orbital energies (epsilon LUMO) for polychlorodibenzofurans and polychlorodibenzo-p-dioxins. Anion abundances were measured using standard mass spectrometric techniques, while epsilon LUMO were calculated by the 'Complete Neglect of Differential Overlap' method. Polychlorodibenzofurans with calculated epsilon LUMO greater than or equal to 1.6 eV show 0% molecular radical anion and those with epsilon LUMO less than or equal to 1.4 eV show greater than or equal to 80% molecular radical anion abundance. Similarly, the molecular radical anion is absent for polychlorodibenzo-p-dioxins with calculated epsilon LUMO greater than or equal to 2.0 eV. A trend towards greater molecular radical ion relative abundance appears for 2.0 eV greater than or equal to epsilon LUMO greater than or equal to 1.0 eV and a maximum is reached around 1 eV, whereupon the molecular ion abundance diminishes with lower epsilon LUMO. B/E linked scan analysis indicates that chlorodioxins with epsilon LUMO less than 1 eV give increasing amounts of metastable anions.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170112","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333460","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 16
Fast atom bombardment mass spectrometric analysis of anthracyclines and anthracyclinones. 蒽环类药物和蒽环类药物的快速原子轰击质谱分析。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170109
C Dass, R Seshadri, M Israel, D M Desiderio
{"title":"Fast atom bombardment mass spectrometric analysis of anthracyclines and anthracyclinones.","authors":"C Dass,&nbsp;R Seshadri,&nbsp;M Israel,&nbsp;D M Desiderio","doi":"10.1002/bms.1200170109","DOIUrl":"https://doi.org/10.1002/bms.1200170109","url":null,"abstract":"<p><p>A mass spectral characterization of a set of anthracyclines and anthracyclinones comprised of daunorubicin, adriamycin and their modified analogs was carried out by using negative and positive fast atom bombardment (FAB) ionization techniques. Addition of more than one hydrogen to the molecular ions of the anthracyclines was observed. The choice of the FAB matrix played an important role in the characterization of these compounds. The dominant ions in the molecular ion region were M-. (or M+.) and MH- (or MH+.2) when sulfolane and glycerol, respectively, were employed as the FAB solvents. The major fragmentation was cleavage of the glycosidic bond with the charge retention mainly on the aglycone moiety. Aromatization of the tetracyclic ring promoted further fragmentation of the aglycone moiety. The anthracyclinones could be characterized only by negative FAB ionization using sulfolane as the FAB matrix. The assigned fragmentation pathways were confirmed by acquiring metastable ion spectra using B/E linked-field scans.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170109","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333457","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 26
The electron impact mass spectra of di- and trinitrofluoranthenes. 二硝基和三硝基氟蒽的电子冲击质谱。
Biomedical & environmental mass spectrometry Pub Date : 1988-07-01 DOI: 10.1002/bms.1200170111
T Ramdahl, B Zielinska, J Arey, R W Kondrat
{"title":"The electron impact mass spectra of di- and trinitrofluoranthenes.","authors":"T Ramdahl,&nbsp;B Zielinska,&nbsp;J Arey,&nbsp;R W Kondrat","doi":"10.1002/bms.1200170111","DOIUrl":"https://doi.org/10.1002/bms.1200170111","url":null,"abstract":"<p><p>The fragmentation pathways of a series of 18 dinitrofluoranthenes (DNF) and four trinitrofluoranthenes have been studied under electron impact conditions. In general, multiple losses of NO2, NO and CO from the molecular ion were observed. Quinonoid ions were observed in the spectra of DNF containing conjugated nitro groups. In addition, some unique fragmentation pathways were detected in the ortho-substituted 1,2- and 2,3-DNF and in the peri-substituted 3,4-DNF.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170111","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14333459","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 6
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