Biomedical & environmental mass spectrometry最新文献

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Dimethylisopropylsilyl ether derivative in gas chromatography/mass spectrometry of 11-dehydrothromboxane B2. 11-脱氢血栓素B2的二甲基异丙基硅醚衍生物气相色谱/质谱分析。
Biomedical & environmental mass spectrometry Pub Date : 1989-11-25 DOI: 10.1248/CPB.37.3015
M. Ishibashi, K. Watanabe, N. Harima, S. Krolik
{"title":"Dimethylisopropylsilyl ether derivative in gas chromatography/mass spectrometry of 11-dehydrothromboxane B2.","authors":"M. Ishibashi, K. Watanabe, N. Harima, S. Krolik","doi":"10.1248/CPB.37.3015","DOIUrl":"https://doi.org/10.1248/CPB.37.3015","url":null,"abstract":"The mass spectrum exhibited a series of ions characteristic of the expected 11-dehydrothromboxane B2 (11-dehydro-TXB2) derivative. Many of the fragmentation products could be explained in terms of simple bond fission mechanisms. A further series of fragmentations proceeded via a six-membered ring transition state or by formation of the cyclic dimethylsilylene ring system. These produced ions in the low mass region containing silicon atoms, characteristic of the protected C-11 carboxylic and moiety. The appearance of these ions may be used for the identification of 11-dehydro-TXB2 and its metabolites having a lactone ring. Six homologue and analogue derivatives were prepared for investigation of the fragmentation mechanism. The proposed fragmentation mechanisms have been supported by accurate mass measurement and mass analyzed ion kinetic energy mass spectrometry.","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1989-11-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85041428","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
Determination of the new aromatic retinoic acid Ro 13-7410 in plasma by two-dimensional gas chromatography negative ion chemical ionization mass spectrometry with selected-ion monitoring. 选择离子监测的二维气相色谱-负离子化学电离质谱法测定血浆中新型芳香族维甲酸Ro 13-7410。
Biomedical & environmental mass spectrometry Pub Date : 1989-07-01 DOI: 10.1002/bms.1200180703
H J Egger, U B Ranalder, E U Koelle, M Klaus
{"title":"Determination of the new aromatic retinoic acid Ro 13-7410 in plasma by two-dimensional gas chromatography negative ion chemical ionization mass spectrometry with selected-ion monitoring.","authors":"H J Egger,&nbsp;U B Ranalder,&nbsp;E U Koelle,&nbsp;M Klaus","doi":"10.1002/bms.1200180703","DOIUrl":"https://doi.org/10.1002/bms.1200180703","url":null,"abstract":"<p><p>A highly sensitive and specific method for the determination of the aromatic retinoic acid Ro 13-7410 in plasma at the picogram per millilitre level is described. The method involves extraction of plasma using Extrelut-1 columns, purification of the extract with Bond Elut-NH2 cartridges, derivatization with pentafluorobenzyl bromide, and subsequent analysis by two-dimensional capillary gas chromatography using the zone-cutting technique, stable isotope dilution and selective negative ion monitoring chemical ionization mass spectrometry. A tetradeuterated analogue is used as internal standard. Quantification is possible down to 25 pg/ml using 1 ml of plasma. The coefficients of variation of the method as calculated from quality control samples are 8.5 and 4.2% at the 100 and 400 pg/ml levels. The method has been applied to the analysis of plasma of volunteers following an oral dose of 40 micrograms Ro 13-7410 and plasma of dogs following an intravenous and oral dose of 25 and 50 micrograms, respectively.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1989-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200180703","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"13914121","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: 10
Deuterated ritanserin analysis by gas chromatography/mass spectrometry: a sensitive technique to study human ritanserin pharmacokinetics. 气相色谱/质谱法分析氘化利坦色林:一种研究人利坦色林药动学的灵敏技术。
Biomedical & environmental mass spectrometry Pub Date : 1989-07-01 DOI: 10.1002/bms.1200180709
P Timmerman, R Woestenborghs, H Lenoir, J Heykants
{"title":"Deuterated ritanserin analysis by gas chromatography/mass spectrometry: a sensitive technique to study human ritanserin pharmacokinetics.","authors":"P Timmerman,&nbsp;R Woestenborghs,&nbsp;H Lenoir,&nbsp;J Heykants","doi":"10.1002/bms.1200180709","DOIUrl":"https://doi.org/10.1002/bms.1200180709","url":null,"abstract":"<p><p>Ritanserin, a new selective serotonin-S2 antagonist, was labelled in one 4-fluorophenyl moiety to obtain a (2H4)-labelled analogue having the following isotopic distribution: 2H0: 0.0%, 2H1: 0.1%, 2H2: 1.9%, 2H3: 5.8%, 2H4: 92.2%. (2H0/2H4) Ritanserin and the internal standard were isolated from the plasma by liquid/liquid extraction and analysed by selected-ion monitoring gas chromatography/mass spectrometry in the 70 eV electron impact mode. A detection limit of 0.1 ng ml-1 could be obtained for both (2H0) and (2H4)ritanserin. The precision (per cent coefficient of variation) and accuracy (per cent relative error) of the method were 4.1% and 4.1%, respectively. The method was used to determine the plasma levels of ritanserin and tetradeuterated ritanserin in three healthy male subjects receiving an equimolar mixture of 5:5 mg (2H0/2H4)ritanserin. The pharmacokinetics of both isotopomers proved to be identical, indicating the absence of an isotope effect, so that this technique might be very promising for use in bioequivalence studies.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1989-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200180709","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"13650578","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: 1
Identification and determination of tert-alkylphenols in carp from the Trenton Channel of the Detroit River, Michigan, USA. 美国密歇根州底特律河特伦顿海峡鲤鱼中叔烷基酚的鉴定与测定。
Biomedical & environmental mass spectrometry Pub Date : 1989-07-01 DOI: 10.1002/bms.1200180706
H Shiraishi, D S Carter, R A Hites
{"title":"Identification and determination of tert-alkylphenols in carp from the Trenton Channel of the Detroit River, Michigan, USA.","authors":"H Shiraishi,&nbsp;D S Carter,&nbsp;R A Hites","doi":"10.1002/bms.1200180706","DOIUrl":"https://doi.org/10.1002/bms.1200180706","url":null,"abstract":"<p><p>Whole carp from the Detroit River were analyzed by gas chromatographic mass spectrometry. Seven tertiary alkyl phenols (tert-pentylphenols, tert-butyl-tert-pentylphenols, a di-tert-pentylphenol and a tri-tert-pentylphenol) and eight chlorinated derivatives of these compounds were identified from their mass spectra and confirmed with synthesized authentic standards. 2,4-Di-tert-pentylphenol was the most abundant of these compounds; in one fish sample, its concentration was about 140 ppm. The same alkyl phenols were also found in technical-grade 2,4-di-tert-pentylphenol, which is manufactured at a chemical plant located near the Detroit River. Comparison of the alkyl phenol levels in carp with those in nearby sediments showed that many of these compounds are taken up by carp and that carp can be used to roughly track local sediment contamination.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1989-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200180706","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"13914123","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: 35
Stable isotope dilution analysis of n-hexanoylglycine, 3-phenylpropionylglycine and suberylglycine in human urine using chemical ionization gas chromatography/mass spectrometry selected ion monitoring. 化学电离气相色谱/质谱选择离子监测分析人尿中正己甘氨酸、3-苯基丙酰甘氨酸和亚基甘氨酸的稳定同位素稀释。
Biomedical & environmental mass spectrometry Pub Date : 1989-07-01 DOI: 10.1002/bms.1200180705
P Rinaldo, J J O'Shea, R D Welch, K Tanaka
{"title":"Stable isotope dilution analysis of n-hexanoylglycine, 3-phenylpropionylglycine and suberylglycine in human urine using chemical ionization gas chromatography/mass spectrometry selected ion monitoring.","authors":"P Rinaldo,&nbsp;J J O'Shea,&nbsp;R D Welch,&nbsp;K Tanaka","doi":"10.1002/bms.1200180705","DOIUrl":"https://doi.org/10.1002/bms.1200180705","url":null,"abstract":"<p><p>We describe a gas chromatographic/mass spectrometric method for the accurate determination of n-hexanoylglycine, 3-phenylpropionylglycine and suberylglycine in urine for the diagnosis of hereditary medium-chain acyl-CoA dehydrogenase (MCAD) deficiency. These acylglycines had previously been detected in urine from patients with MCAD deficiency, but their diagnostic values were unknown because of a lack of appropriate analytical methods. n-Hexanoyl(1,2-13C)glycine, 3-phenylpropionyl(2-13C,15N)glycine and suberyl(2-13C,15N)glycine were synthesized and used as internal standards. Ammonia chemical ionization was utilized to generate intense [M + H]+ ions for selected-ion monitoring quantification. The whole procedure is fast and can be performed by a low-resolution gas chromatographic/mass spectrometric system, giving accurate results over a range of three orders of magnitude (0.0167-16.7 micrograms/ml). The results from the analyses of 54 urine samples from 21 MCAD-deficient patients and various control samples using this method established that n-hexanoyglycine and 3-phenylpropionylglycine were highly diagnostic for this disease, while suberylglycine was found less specific.</p>","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1989-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200180705","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"13914122","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: 23
A rapid liquid-solid extraction procedure for the quantification of clenbuterol in urine. 快速液固萃取法定量测定尿中盐酸克仑特罗。
Biomedical & environmental mass spectrometry Pub Date : 1988-11-01 DOI: 10.1002/bms.1200170512
J Schmid, A Bücheler
{"title":"A rapid liquid-solid extraction procedure for the quantification of clenbuterol in urine.","authors":"J Schmid,&nbsp;A Bücheler","doi":"10.1002/bms.1200170512","DOIUrl":"https://doi.org/10.1002/bms.1200170512","url":null,"abstract":"","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170512","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14337822","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: 10
Quantitation of clenbuterol in biological fluids using ammonia CI and automated capillary GCMS. 氨CI和自动毛细管气相色谱法定量生物体液中的克仑特罗。
Biomedical & environmental mass spectrometry Pub Date : 1988-11-01 DOI: 10.1002/bms.1200170513
H J Förster, K L Rominger, E Ecker, H Peil, A Wittrock
{"title":"Quantitation of clenbuterol in biological fluids using ammonia CI and automated capillary GCMS.","authors":"H J Förster,&nbsp;K L Rominger,&nbsp;E Ecker,&nbsp;H Peil,&nbsp;A Wittrock","doi":"10.1002/bms.1200170513","DOIUrl":"https://doi.org/10.1002/bms.1200170513","url":null,"abstract":"","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1002/bms.1200170513","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14337826","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: 19
Proceedings of the International Symposium on Applied Mass Spectrometry in the Health Sciences. Barcelona, Spain, 28-30 September 1987. 质谱在健康科学中的应用国际研讨会论文集。1987年9月28日至30日,西班牙巴塞罗那。
{"title":"Proceedings of the International Symposium on Applied Mass Spectrometry in the Health Sciences. Barcelona, Spain, 28-30 September 1987.","authors":"","doi":"","DOIUrl":"","url":null,"abstract":"","PeriodicalId":8924,"journal":{"name":"Biomedical & environmental mass spectrometry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1988-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14370820","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: 0
Measurement of phenylacetic acid in cerebrospinal fluid and plasma using combined gas chromatography/electron capture chemical ionization mass spectrometry. 联合气相色谱/电子俘获化学电离质谱法测定脑脊液和血浆中的苯乙酸。
Biomedical & environmental mass spectrometry Pub Date : 1988-09-01 DOI: 10.1002/bms.1200170310
K F Faull, N Pascoe, K A Greene, J F Maddaluno, J Lunde, R J King
{"title":"Measurement of phenylacetic acid in cerebrospinal fluid and plasma using combined gas chromatography/electron capture chemical ionization mass spectrometry.","authors":"K F Faull,&nbsp;N Pascoe,&nbsp;K A Greene,&nbsp;J F Maddaluno,&nbsp;J Lunde,&nbsp;R J King","doi":"10.1002/bms.1200170310","DOIUrl":"https://doi.org/10.1002/bms.1200170310","url":null,"abstract":"<p><p>Details are presented of an ultra-sensitive gas chromatographic/mass spectrometric assay for phenylacetic acid in plasma and cerebrospinal fluid based on measurements of the relative intensities of the carboxylate anions, derived from the penta- and tetrafluorobenzyl esters under electron capture chemical ionization conditions, of unlabeled and a (13C2)-labeled internal standard. The limits of detection for the penta- and tetrafluorobenzyl esters are 0.85 and 4.0 pg respectively, and the assay is capable of measuring phenylacetic acid concentrations in samples as small as 20 microliter of CSF and plasma. The penta- and tetrafluorobenzyl esters are chromatographically separated on the gas chromatograph column, which allows for their co-injection and independent measurement from the same chromatogram.</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.1200170310","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14345577","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: 9
Potassium ion ionization of desorbed species (K+IDS): a rapid method for the screening of urine for organic acidemias. 解吸态钾离子电离(K+IDS):一种快速筛选尿液有机酸血症的方法。
Biomedical & environmental mass spectrometry Pub Date : 1988-09-01 DOI: 10.1002/bms.1200170311
D B Kassel, J Allison
{"title":"Potassium ion ionization of desorbed species (K+IDS): a rapid method for the screening of urine for organic acidemias.","authors":"D B Kassel,&nbsp;J Allison","doi":"10.1002/bms.1200170311","DOIUrl":"https://doi.org/10.1002/bms.1200170311","url":null,"abstract":"<p><p>A new desorption/ionization mass spectrometric technique, K+ ionization of desorbed species (K+IDS), is evaluated as a rapid method for differentiating various organic acidemias, conditions in which excessive levels of organic acid metabolites are present in plasma or urine as a result of some inborn error of metabolism. This method requires no derivatization of the isolated organic acids, unlike that required for gas chromatographic and gas chromatographic/mass spectrometric analyses. 'Batch' mass spectrometric analysis is achieved by deposition of the complex organic acid mixture (from urine) onto a K+IDS probe. Rapid heating results in the emission of alkali ions (Na+ or K+) from a thermionic emitter and the intact desorption of analyte. Subsequent gas-phase addition produces a mass spectrum showing alkali ion adducts of the components, providing molecular weight and relative concentration information. This rapid desorption/ionization technique requires no matrix, and analysis times are exceedingly short relative to those required in gas chromatographic/mass spectrometric analyses. Results suggest that differential diagnosis of some of the more commonly occurring organic acidemias (e.g. isovaleric acidemia, maple syrup urine disease, etc.) may be made.</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.1200170311","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"14345578","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: 4
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