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电喷雾质谱结合化学计量学方法快速筛选玛咖促睾丸间质细胞增殖活性成分 总被引:2,自引:0,他引:2
应用电喷雾串联质谱法( ESI-MS/MS)对云南和秘鲁产玛咖样品中低极性化学成分进行检测,获得各样品的一级质谱指纹谱图和各离子峰的二级质谱数据,并测定各样品促进大鼠睾丸间质细胞增殖活性,采用化学计量学方法主成分分析( PCA)、偏最小二乘法( PLS)和灰色关联度分析( GRA)对所获得的一级质谱数据进行处理后,可有效区分玛咖的不同产地,且筛选出其中具有促大鼠睾丸间质细胞增殖活性的可能成分,进而通过二级质谱数据分析得到可能活性成分的结构。实验结果表明,玛咖低极性成分具有很好的促大鼠睾丸间质细胞增殖活性,其中活性较强的主要为N-benzylhexadecanamide和N-benzy-(9Z,12Z,15Z)-octadecatrien-amide。本方法为简单、快速分析中药中促睾丸间质细胞增殖活性成分筛选方法提供了借鉴。 相似文献
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超高效液相色谱-电喷雾串联质谱测定蔬菜中喹诺酮类抗生素 总被引:5,自引:0,他引:5
建立了蔬菜中4种喹诺酮类抗生素的超高效液相色谱-电喷雾串联质谱(UPLC-ESI-MS/MS)分析方法。每克蔬菜样品(干重)以15 mL乙腈-HCl(125∶8,V/V)进行振荡-超声提取3次,用HLB固相萃取柱进行净化富集,以6 mL 1%酸化乙腈进行洗脱,用N2进行吹脱,最后用初始流动相进行定容。以0.1%甲酸-乙腈溶液和0.1%甲酸溶液作为流动相,采用梯度洗脱方式进行UPLC-ESI-MS/MS检测。蔬菜中4种喹诺酮类化合物不同浓度加标回收率为61%~90%;相对标准偏差(RSD)小于5%(个别除外);检出限为0.021~0.092μg/kg;定量限为0.065~0.312μg/kg。本方法能够满足实际蔬菜样品的分析要求。 相似文献
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采用超高效液相色谱-电喷雾串联四极杆质谱仪(UPLC-ESI-MS/MS)同时测定蜂胶保健品中14种活性成分和9种违禁降糖西药。蜂胶保健品样品用甲醇稀释,超声波提取,样品溶液经高速离心后过滤。使用ACQUITY UPLC C18反相柱(50 mm×2.1 mm,1.7μm);流动相为0.3%甲酸溶液和乙腈,在梯度条件下分析,目标分析物在多反应监测(MRM)模式下以保留时间和离子对(母离子和两个碎片离子)信息比较进行定性和定量分析。本方法的活性成分检出限(LOD)为0.7~42.0 mg/kg;定量限(LOQ)为2.2~140 mg/kg;活性成分的加标回收率为77.8%~113.6%;违禁降糖西药的LOD为0.1~0.9 mg/kg,LOQ为0.3~2.5 mg/kg;违禁降糖西药的平均回收率为79.3%~108.5%。本方法简便、有效、灵敏,为评价蜂胶保健品质量提供了新的检测方法。 相似文献
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高效液相色谱-电喷雾飞行时间质谱分析娑罗子中皂苷类成分 总被引:8,自引:0,他引:8
采用高效液相色谱/电喷雾飞行时间质谱联用技术(HPLC/ESI-TOF/MS),研究4种七叶皂苷的分子结构与裂解规律间的关系,并对娑罗子中的七叶皂苷类化合物进行鉴定。实验采用反相C18色谱柱,以乙腈-0.2%乙酸溶液为流动相,二元线性梯度洗脱,通过与电喷雾飞行时间质谱联用获得娑罗子中各皂苷成分的精确分子量和分子式;采用质谱碰撞诱导解离技术获得各化合物碎片裂解信息,结合文献对娑罗子中的14种皂苷类化合物进行了初步鉴定。研究表明,高效液相色谱-电喷雾飞行时间质谱联用技术是娑罗子中皂苷类化合物鉴别的有效工具。 相似文献
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Cheguillaume G Buchmann W Desmazières B Tortajada J 《Journal of mass spectrometry : JMS》2004,39(4):368-377
Two model peptides, des-Arg1-bradykinin (DAB) and bradykinin (B), were cationized by Ag+ after their separation by reversed-phase liquid chromatography (RPLC) prior to mass spectrometry (MS). Silver nitrate solution was used as a post-column reagent. The RPLC and MS experimental conditions were optimized using flow injection in order to obtain sufficiently abundant silver adducts to permit MS/MS experiments. The use of water-methanol with 0.1% formic acid as mobile phase allowed a good chromatographic separation of the two peptides with a polymeric stationary phase and sufficiently abundant silver-containing adducts, [M + Ag + H]2+ and [M + 2Ag]2+. The gas-phase dissociation of [DAB + Ag + H]2+ and [DAB + 2Ag]2+ led to interpretable mass spectra during the on-line cationization experiment. Most of the ions obtained by dissociating [DAB + Ag + H]2+ and [DAB + 2Ag]2+ species are silver-containing ions but the ions produced depend on the parent. The ions coming from the dissociation of the doubly charged silver adducts [DAB + Ag + H]2+ or [DAB + 2Ag]2+ are of interest compared with those coming from the singly charged silver species or doubly charged protonated species. The fragmentation of the doubly charged silver adducts provides ions over the entire mass range. Although the presence of several prolines in des-Arg1-bradykinin prevents the formation of some expected ions, the observation of triplets [an-H + Ag]+, [bn-H + Ag]+ and [bn + OH + Ag]+ produced by the dissociation of on-line Ag(+)-cationized peptides could contribute to greater success of automatic sequencing of peptides. 相似文献
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Analytical methods were developed for atorvastatin, novobiocin and roxithromycin using microbore liquid chromatography/electrospray ionization tandem mass spectrometry (microbore LC/ESI-MS/MS) in positive and negative voltage switching mode. Atorvastatin and roxithromycin require the positive-ion mode, whereas the negative-ion mode is required for the determination of novobiocin. Using the positive and negative voltage switching function, the three analytes were determined with one injection, and the time required was half that required using separately run positive- and negative-ion modes, without any reduction in sensitivity. A microbore LC column (100 x 1.0 mm i.d.) was chosen for chromatographic separation with mobile phase solvents acetonitrile and 10 mM aqueous ammonium acetate. The flow-rate was 0.1 ml min(-1) and the injection volume was 1 micro l. The analytes were quantified in the multiple reaction monitoring mode with external standards. By switching the positive and negative voltage, the three analytes were determined with a 4 min chromatographic run and with instrumental detection limits of 1-3 pg. This analytical method, using a microbore LC column combined with solid-phase extraction, was applied successfully to the determination of trace levels of the above pharmaceuticals in aqueous samples. Atorvastatin was detected in a sewage treatment plant final effluent. 相似文献
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A liquid chromatographic/tandem mass spectrometric (LC/MS/MS) screening method was developed for the screening of 11 calcium channel blockers of the 1,4-dihydropyridine type in plasma samples for forensic and clinical cases. Plasma samples were extracted by automated solid-phase extraction. Analysis was performed using a reversed-phase C(18) column, gradient elution and a triple-quadrupole mass spectrometer with TurboIonSpray source in positive mode and multiple reaction monitoring. This method was found to be selective and sensitive for the detection of the target compounds at their therapeutic plasma concentrations. 相似文献
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Xu DH Lou HG Yuan H Jiang B Zhou Q Zhang ZM Ruan ZR 《Biomedical chromatography : BMC》2008,22(4):433-440
A simple and sensitive liquid chromatography-tandem mass spectrometry method was developed and validated for determining domperidone in human plasma. The analyte and internal standard (IS; mosapride) were isolated from plasma samples by protein precipitation with methanol (containing 0.1% formic acid). The chromatographic separation was performed on an Xterra MS C(18) Column (2.1 x 150 mm, 5.0 microm) with a gradient programme mobile phase consisting of 0.1% formic acid and acetonitrile at a flow rate of 0.30 mL/min. The total run time was 4.0 min. The analyses were carried out by multiple reaction monitoring using the parent-to-daughter combinations m/z 426 --> 175 and m/z 422 --> 198 (IS). The areas of peaks from the analyte and IS were used for quantification of domperidone. The method was validated according to the FDA guidelines on bioanalytical method validation. Validation results indicated that the lower limit of quantification was 0.2 ng/mL, and the assay exhibited a linear range of 0.2-60.0 ng/mL and gave a correlation coefficient (r(2)) of 0.999 or better. Quality control samples (0.4, 0.8, 15 and 50 ng/mL) in six replicates from three different analytical runs demonstrated an intra-assay precision (RSD) 4.43-6.26%, an inter-assay precision 5.25-7.45% and an overall accuracy (relative error) of <6.92%. The method can be applied to pharmacokinetic and bioequivalence studies of domperidone. 相似文献
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Brian D. McGarvey Hui Liao Keyi Ding Xiaoling Wang 《Journal of mass spectrometry : JMS》2012,47(6):687-693
In the search for novel natural products in plants, particularly those with potential bioactivity, it is important to efficiently distinguish novel compounds from previously isolated, known compounds, a process known as dereplication. In this study, electrospray ionization‐multiple stage tandem mass spectrometry (ESI‐MSn) was used to study the behaviour of 12 pregnane glycosides and genins previously isolated from Marsdenia tenacissima, a traditional Chinese medicinal plant, as a basis for dereplication of compounds in a plant extract. In addition to [M + Na]+ and [M + NH4]+ ions, a characteristic [M‐glycosyl + H]+ ion was observed in full‐scan mode with in‐source fragmentation. Sequential in‐trap collision‐induced dissociation of [M + Na]+ ions from 11,12‐diesters revealed consistent preferred losses of substituents first from C‐12, then from C‐11, followed by losses of monosaccharide fragments from the C‐3 tri‐ and tetrasaccharide substituents. A crude methanol extract of M. tenacissima stems was analysed using high‐performance liquid chromatography coupled to ESI‐MS. Several previously isolated pregnane glycosides were dereplicated, and the presence of an additional nine novel pregnane glycosides is predicted on the basis of the primary and fragment ions observed, including two with a previously unreported C4H7O C‐11/C‐12 substituent of pregnane glycosides. This study is the first report of prediction of the structures of novel pregnane glycosides in a crude plant extract by a combination of in‐source fragmentation and in‐trap collision‐induced dissociation and supports the usefulness of LC‐ESI‐MSn not only for dereplication of active compounds in extracts of medicinal plants but also for detecting the presence of novel related compounds. Copyright © 2012 John Wiley & Sons, Ltd. 相似文献
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Mazzuca P Ferranti P Picariello G Chianese L Addeo F 《Journal of mass spectrometry : JMS》2005,40(1):83-90
A mass spectrometric-based procedure for anthocyanin profiling was set up to distinguish authentic Vitis vinifera from hybrid red grapevine cultivars. 3-O-Monoglucoside and the related acetyl-, p-coumaryl- and caffeoyl-monoglucoside anthocyanins occurred only in Vitis vinifera, whereas 3,5-O-diglucoside and the substituted acetyl-, p-coumaryl-, feruloyl- and caffeoyl-diglucoside anthocyanins were the additional pigments in hybrid grapevines. The procedure was applied expressly to identify red grape cultivars based on the anthocyanin chemo-type determination. In particular, a red grape cultivar, having 3,5-O-diglucoside anthocyanins and a novel class of anthocyanin monoglucosides, such as cyanidin-3-O-, cyanidin-3-O-(6-O-acetyl)- and cyanidin-3-O-(6-O-p-coumaryl)pentoside, was classified as hybrid. A second vine cultivar, characterized exclusively by 3-O-monoglucoside anthocyanins, was included among the Vitis vinifera species. Anthocyanin profiling by mass spectrometry could represent the core of a chemotaxonomic procedure for distinguishing American and European grapevines based on the identification of post-synthetic anthocyanidin modification. 相似文献
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Eunju Cha Sohee Kim Hee Won Kim Kang Mi Lee Ho Jun Kim Oh‐Seung Kwon Jaeick Lee 《Biomedical chromatography : BMC》2016,30(4):555-565
The relationships between the ionization profile, sensitivity, and structures of 64 exogenous anabolic steroids (groups I–IV) was investigated under electrospray ionization (ESI) conditions. The target analytes were ionized as [M + H]+ or [M + H–nH2O]+ in the positive mode, and these ions were used as precursor ions for selected reaction monitoring analysis. The collision energy and Q3 ions were optimized based on the sensitivity and selectivity. The limits of detection (LODs) were 0.05–20 ng/mL for the 64 steroids. The LODs for 38 compounds, 14 compounds and 12 compounds were in the range of 0.05–1, 2–5 and 10–20 ng/mL, respectively. Steroids including the conjugated keto‐functional group at C3 showed good proton affinity and stability, and generated the [M + H]+ ion as the most abundant precursor ion. In addition, the LODs of steroids using the [M + H]+ ion as the precursor ion were mostly distributed at low concentrations. In contrast, steroids containing conjugated/unconjugated hydroxyl functional groups at C3 generated [M + H ? H2O]+ or [M + H ? 2H2O]+ ions, and these steroids showed relatively high LODs owing to poor stability and multiple ion formation. An LC‐MS/MS method based on the present ionization profile was developed and validated for the determination of 78 steroids (groups I–V) in human urine. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
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A method for the quantification of clindamycin in animal plasma using high-performance liquid chromatography combined with electrospray ionization mass spectrometry (LC/ESI-MS/MS) is presented. Lincomycin is used as the internal standard. The sample preparation includes a simple deproteinization step with trichloroacetic acid. Chromatographic separation is achieved on an RP-18 Hypersil column using gradient elution with 0.01 M ammonium acetate and acetonitrile as mobile phase. Good linearity was observed in the range 0-10 microg ml(-1). The limit of quantification of the method is 50 ng ml(-1) and the limit of detection is 1.3 ng ml(-1). The method was shown out to be of use for pharmacokinetic studies of clindamycin formulations in dogs. 相似文献
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Maes A Meyns T Sustronck B Maes D De Backer P Croubels S 《Journal of mass spectrometry : JMS》2007,42(5):657-663
The aim of this study was to develop a rapid and sensitive method for the quantification of cefquinome in animal plasma and bronchoalveolar lavage (BAL) fluid using high-performance liquid chromatography combined with electrospray tandem mass spectrometry (LC-ESI-MS/MS). Cefadroxil is used as internal standard. For plasma, the sample preparation includes a simple deproteinization step with a Microcon filter. This allows detecting the unbound cefquinome concentration, which is correlated with the concentration in other body fluids, such as BAL fluid. To be able to detect the total plasma concentration, deproteinization with acetonitrile, followed by a back-extraction of actonitrile with dichloromethane was performed. The BAL fluid is centrifuged to precipitate floating particles. Chromatographic separation is achieved on a PLRP-S column using 0.005% formic acid and methanol as mobile phase. For plasma, good linearity was observed in the range of 5-2500 ng ml(-1) for both the unbound and total concentration. The response in BAL fluid was linear in the range of 4-1000 ng ml(-1). The limit of quantification (LOQ) was set at 5.00 ng ml(-1) for plasma and at 4.00 ng ml(-1) for BAL fluid. The limit of detection (LOD) was 3.12 ng ml(-1) and 0.41 ng ml(-1) for the unbound and total concentration in plasma, respectively, and was 1.43 ng ml(-1) for BAL fluid. The method was shown to be of use in a pharmacokinetic study in pigs, where the correlation between cefquinome concentrations in plasma and BAL fluid of pigs was studied. 相似文献
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A novel, sensitive and specific method for the quantitative determination of ivermectin B(1a) in animal plasma using liquid chromatography combined with positive electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) is presented. Abamectin was used as the internal standard. Extraction of the samples was performed with a deproteinization step using acetonitrile. Chromatographic separation was achieved on a Nucleosil ODS 5 microm column, using gradient elution with 0.2% (v/v) acetic acid in water and 0.2% (v/v) acetic acid in acetonitrile. The method was validated according to the requirements defined by the European Community. Calibration curves using plasma fortified between 1 and 100 ng ml(-1) showed a good linear correlation (r > or = 0.9989, goodness-of-fit coefficient < or =8.1%). The trueness at 2 and 25 ng ml(-1) (n = 6) was +4.2 and -17.1%, respectively. The trueness and between-run precision for the analysis of quality control samples at 25 ng ml(-1) was -4.0 and 11.0%, respectively (n = 16). The limit of quantification of the method was 1.0 ng ml(-1), for which the trueness and precision also fell within acceptable limits. Using a signal-to-noise ratio of 3 : 1, the limit of detection was calculated to be 0.2 ng ml(-1). The specificity was demonstrated with respect to ivermectin B(1b).The method was successfully used for the quantitative determination of ivermectin B(1a) in plasma samples from treated bovines, demonstrating the usefulness of the developed method for application in the field of pharmacokinetics. 相似文献