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Determination of urine catecholamines and metanephrines by reversed-phase liquid chromatography-tandem mass spectrometry 被引量:6
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作者 CHEUK Man-Yung LO Yun-Chuen POON Wing-Tat 《色谱》 CAS CSCD 北大核心 2017年第10期1042-1047,共6页
The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tande... The measurement of urine catecholamine and metanephrine concentrations is important for biochemical screening and diagnosis of pheochromocytoma.The goal of this work was to develop a simple liquid chromatography-tandem mass spectrometry(LC-MS/MS)method for determining catecholamines and metanephrines in urine to replace an existing liquid chromatographic method using electrochemical detection.Urine samples were prepared using Oasis weak-cation-exchange cartridges.The eluate was analyzed on an Agilent ZORBAX Eclipse Plus Phenyl-Hexyl column in 3 min.Adrenaline,noradrenaline,dopamine,metanephrine,normetanephrine,and their deuterated internal standards were monitored in positive electrospray ionization mode by multiple reaction monitoring(MRM).No evidence of ion suppression was observed.The assay was linear up to 5μmol/L for adrenaline,5μmol/L for noradrenaline,6.1μmol/L for dopamine,5.6μmol/L for metanephrine,and 34.6μmol/L for normetanephrine,with lower limits of quantification of 5,5,12,6 and 7nmol/L,respectively.The intra-day and inter-day precisions for all analytes ranged from 0.59%to 4.64%and1.98%to 4.80%,respectively.External quality assurance samples were assayed and showed excellent agreement with the target values.This simple method provides an improved assay for determining urine catecholamines and metanephrines. 展开更多
关键词 liquid chromatography-tandem mass spectrometry (LC-MS/MS) METANEPHRINES CATECHOLAMINES PHEOCHROMOCYTOMA URINE
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Simultaneous determination of 15 pesticide residues in Chinese cabbage and cucumber by liquid chromatography-tandem mass spectrometry utilizing online turbulent flow chromatography 被引量:5
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作者 Sufang Fan Junmei Ma +5 位作者 Meirong Cao Juan Wang Leilei Zhang Yan Zhang Qiang Li Jia Chen 《Food Science and Human Wellness》 SCIE 2021年第1期78-86,共9页
In this experiment,a liquid chromatography tandem mass spectrometry method was built to determine 15 pesticide residues in Chinese cabbage and cucumber samples based on online turbulent flow chromatography purificatio... In this experiment,a liquid chromatography tandem mass spectrometry method was built to determine 15 pesticide residues in Chinese cabbage and cucumber samples based on online turbulent flow chromatography purification.After modified quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction,extracts were directly injected to the TLX(TurboFlow Liquid Xcalibur)system and brought to TurboFlow™columns for on-line purification and then transferred to analytical column for further separation and analysis.TurboFlow™columns types,transfer flow rate,and transfer time were optimized.Limits of detection and limits of quantification of the method obtained for 15 pesticide residues were ranged between 0.2–1.0μg/kg and 0.5–2.0μg/kg in Chinese cabbage and cucumber samples.Recoveries of pesticide residues were in range of 75.3%–103.7%.Matrix effects for 15 pesticides were in range of 5.6%–106.6%.The developed method has been successfully used for the determination of 15 pesticide residues in real samples. 展开更多
关键词 Pesticide residues Online turbulent flow chromatography Liquid chromatography-tandem mass spectrometry
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Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry
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作者 Lech RODZIEWICZ Jolanta MASLOWIECKA +1 位作者 Anna SADOWSKA Halina CAR 《色谱》 CAS CSCD 北大核心 2017年第10期1048-1054,共7页
Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC... Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine. 展开更多
关键词 ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) thyreostats (TSs) URINE
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Determination of egg and milk allergen in food products by liquid chromatography-tandem mass spectrometry based on signature peptides and isotope-labeled internal standard
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作者 Sufang Fan Junmei Ma +4 位作者 Zhuo Liu Yawei Ning Meicong Cao Qiang Li Yan Zhang 《Food Science and Human Wellness》 SCIE CSCD 2023年第3期728-736,共9页
The aim of this work was to develop a liquid chromatography-tandem mass spectrometry method for the determination of milk allergen and egg allergen in food products.Signature peptides GGLEPINFQTAADQAR,VGINYWLAHK,VLVLD... The aim of this work was to develop a liquid chromatography-tandem mass spectrometry method for the determination of milk allergen and egg allergen in food products.Signature peptides GGLEPINFQTAADQAR,VGINYWLAHK,VLVLDTDYK,FFVAPFPEVFGK,and NAVPITPTLNR were confirmed and synthesized as the quantitative peptide of ovalbumin,α-lactalbumin,β-lactoglobulin,α_(S1)-casein andα_(S2)-casein,the relative isotope-labeled internal standards were used in the quantitative analysis.Linear range was in the range of0.5-5000.0 nmol/L for egg and milk allergen in bread,cake,cookie,rice crust and wheat flour samples with free from egg and milk,the limits of detection of milk allergens and egg allergen were in the range between0.94 mg/100 g and 56.71 mg/100 g,limits of quantification of milk allergens and egg allergen were in the range between 2.36 mg/100 g and 141.78 mg/100 g.The recoveries ranged from 76.7%to 122.8%,the relative standard deviations were in the range of 1.60%-15.60%.The developed method has been successfully used for the detection of egg and milk allergen in various food samples. 展开更多
关键词 Liquid chromatography-tandem mass spectrometry Egg and milk allergen Signature peptides Isotope-labeled internal standards
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Identification and the molecular mechanism of novel duck liver-derived anti-inflammatory peptides in lipopolysaccharide-induced RAW264.7 cell model
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作者 Xiankang Fan Laidi Zhang +5 位作者 Yangying Sun Changyu Zhou Qiang Xia Lihui Du Zhen Wu Daodong Pan 《Food Science and Human Wellness》 SCIE CAS CSCD 2024年第6期3595-3605,共11页
In this study,10 novel anti-inflammatory peptides were identified from duck liver,and their molecular mechanism was demonstrated based on machine learning and molecular docking.Using Sephadex G-15 gel chromatography s... In this study,10 novel anti-inflammatory peptides were identified from duck liver,and their molecular mechanism was demonstrated based on machine learning and molecular docking.Using Sephadex G-15 gel chromatography separation,reversed-phase high-performance liquid chromatography purification,liquid chromatography-tandem mass spectrometry identification,and BIOPEP database comparison,10 novel antiinflammatory peptides were initially found.Their splendid angiotensin-converting enzyme(ACE)inhibition and anti-inflammatory properties were confirmed by machine learning.With binding energies less than–20.93 kJ/mol,molecular docking revealed that they could efficiently bind to the active pockets of tumor necrosis factorα(TNF-α),interleukin 6(IL-6),cyclooxygenase 2(COX-2),and nuclear factorκB(NF-κB)proteins with efficiency,indicating that the compounds can spontaneously form complexes through hydrogen bonding and hydrophobic interactions with the protein binding pockets.In the lipopolysaccharide-induced RAW264.7 cell model,the release of NO,TNF-α,and IL-6 and the mRNA expression of inflammatory factors(TNF-α,IL-6,COX-2,and NF-κB)were significantly inhibited by these peptides.We concluded it might be due to their anti-inflammatory effects by inhibiting the protein phosphorylation of inhibitor of NF-κB(IκBα)in the cytoplasm and preventing the translocation of NF-κB p65 in the cytoplasm to the nucleus,thereby regulating the NF-κB signaling pathway.This study is essential for the screening of anti-inflammatory peptides and the investigation of the mechanism of action. 展开更多
关键词 PEPTIDES Machine learning Molecular docking Infl ammation Liquid chromatography-tandem mass spectrometry
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高效液相色谱-串联质谱法对猪肉中四种大环内酯类药物残留量的测定 被引量:6
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作者 夏曦 李晓薇 +3 位作者 江海洋 李建成 安保超 丁双阳 《分析测试学报》 CAS CSCD 北大核心 2008年第S1期224-226,230,共4页
A simple and sensitive method was developed for the simultaneous determination of four macrolides in pork using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Homogenized sample was extrac... A simple and sensitive method was developed for the simultaneous determination of four macrolides in pork using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Homogenized sample was extracted with NaH2PO4 buffer and acetonitrile solution,and defatted with n-hexane.Further cleanup was performed on a Sep-Pakt C18 solid-phase extraction cartridge.The compounds were determined by LC-MS/MS operated in positive electrospray ionization mode.The limits of detection(LODs) were 0.5 μg/kg.The average recoveries at three spiked concentration levels of 1.0,5.0,10.0 μg/kg were in the range of 70%-110%,with the intra-day RSD of less than 12.9% and inter-day RSD of less than 13.4%. 展开更多
关键词 high performance liquid chromatography-tandem mass spectrometry PORK MACROLIDE
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固相萃取-超快速液相色谱-串联质谱法同时测定血液中的4种苏丹染料 被引量:13
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作者 朱浩 黄坤玉 +5 位作者 付建飞 胡岳 黄娴妮 陈晓红 邹宝波 金米聪 《色谱》 CAS CSCD 北大核心 2014年第3期224-229,共6页
建立了血液样品中4种苏丹染料(苏丹Ⅰ、Ⅱ、Ⅲ和Ⅳ)的固相萃取-超快速液相色谱-串联质谱( UFLC-MS /MS)测定方法。样品经乙腈涡旋振荡提取,上清液加等体积水稀释混匀后移入 C18固相萃取小柱净化,采用 Agi-lent Eclipse Plus C18... 建立了血液样品中4种苏丹染料(苏丹Ⅰ、Ⅱ、Ⅲ和Ⅳ)的固相萃取-超快速液相色谱-串联质谱( UFLC-MS /MS)测定方法。样品经乙腈涡旋振荡提取,上清液加等体积水稀释混匀后移入 C18固相萃取小柱净化,采用 Agi-lent Eclipse Plus C18色谱柱(100 mm×2.1 mm,1.8μm)以0.1%(v / v)甲酸水溶液和0.1%(v / v)甲酸乙腈溶液为流动相梯度洗脱分离,电喷雾电离(ESI)正离子多反应监测模式进行定量分析。讨论了苏丹Ⅲ和苏丹Ⅳ的偶氮基团 E-Z 光学异构现象,并对影响因素进行了分析。结果4种苏丹染料在0.1~20.0μg / L 范围内线性关系良好,相关系数均大于0.999;在低、中、高3个加标水平的平均回收率为93.0%~108.2%,相对标准偏差为4.8%~9.5%;方法的检出限(LOD)为0.06μg / L,定量限(LOQ)为0.2μg / L。本方法准确、快速、灵敏,可用于血液样品中苏丹类染料的检测分析。 展开更多
关键词 超快速液相色谱-串联质谱法 固相萃取 苏丹染料 血液 ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS MS) sol-id-phase extraction(SPE)
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液相色谱-串联质谱法测定水环境中的十氯酮 被引量:5
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作者 周丽 董亮 +5 位作者 史双昕 张利飞 张秀蓝 杨文龙 李玲玲 黄业茹 《色谱》 CAS CSCD 北大核心 2014年第3期211-215,共5页
建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后,采用 Eclipse plus C18柱(100 mm×2.1 mm,3.5μm)分离,乙腈和水为流动相进行梯度洗脱,在电喷雾负离子多反应监测模式下进行检测,同位素内标法... 建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后,采用 Eclipse plus C18柱(100 mm×2.1 mm,3.5μm)分离,乙腈和水为流动相进行梯度洗脱,在电喷雾负离子多反应监测模式下进行检测,同位素内标法定量。结果表明:采用液相色谱-质谱联用技术,证实了十氯酮在甲醇中以半缩醛的形式存在,而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强,在净化时难以洗脱,并且不耐酸,所以不能与其他有机氯农药一起分析。十氯酮在5~100μg / L 范围有良好的线性关系,相关系数 r2=0.999,检出限及定量限分别为0.70 ng / L 和2.8 ng / L;在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1%~98.9%,相对标准偏差为3.85%~4.72%。本方法具有良好的灵敏度、回收率和重现性,适用于水环境中十氯酮的测定。 展开更多
关键词 高效液相色谱-串联质谱 十氯酮 high performance liquid chromatography-tandem mass spectrometry( HPLC-MS MS)
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高效液相色谱-串联质谱法测定比格犬血浆中的莫诺苷浓度及其药代动力学 被引量:6
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作者 熊山 李敬来 +3 位作者 朱秀清 王晓英 吕圭源 张振清 《色谱》 CAS CSCD 北大核心 2014年第3期290-293,共4页
运用高效液相色谱-串联质谱联用技术,建立了简单、快速、灵敏的比格犬灌胃莫诺苷后血药浓度的检测方法。血浆样品采用蛋白质沉淀法处理,以芍药苷作为内标,色谱柱为 Inertsil ODS-SP 色谱柱(50 mm ×2.1 mm,5μm),流动相为水... 运用高效液相色谱-串联质谱联用技术,建立了简单、快速、灵敏的比格犬灌胃莫诺苷后血药浓度的检测方法。血浆样品采用蛋白质沉淀法处理,以芍药苷作为内标,色谱柱为 Inertsil ODS-SP 色谱柱(50 mm ×2.1 mm,5μm),流动相为水(含1 mmol / L 甲酸钠)-乙腈,梯度洗脱,流速0.4 mL / min。采用电喷雾离子源( ESI),正离子多反应监测(MRM)模式。绘制血药浓度-时间曲线,并采用 DAS 2.0软件计算药代动力学参数。方法学实验结果表明内源性杂质不干扰莫诺苷和内标的测定,线性范围为2~5000μg / L( r =0.9966),定量限为2μg / L。方法精密度、准确度、回收率和基质效应均符合生物样品测定的要求,适合比格犬血浆中莫诺苷浓度的测定,可以应用该方法进行莫诺苷的药代动力学研究。比格犬灌胃莫诺苷3个剂量(5、15、45 mg / kg)后的血药浓度-时间曲线下面积(AUC(0-∞))分别为(1631.20±238.50)、(3984.05±750.38)、(10397.64±3156.34)μg / L&#183;h,与给药剂量之间呈现良好的线性关系。 展开更多
关键词 液相色谱-串联质谱 莫诺苷 血浆 比格犬 药代动力学 liquid chromatography-tandem mass spectrometry ( LC-MS MS )
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超高效液相色谱-三重四极杆串联质谱法测定柑橘中4种苯甲酰脲类农药残留 被引量:12
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作者 张月 林靖凌 +1 位作者 韩丙军 吕岱竹 《农药学学报》 CAS CSCD 北大核心 2014年第5期614-618,共5页
建立了柑橘中虱螨脲、灭幼脲、氟啶脲和除虫脲4种苯甲酰脲类农药同时检测的超高效液相色谱-三重四级杆串联质谱( UPLC-MS/MS)分析方法。样品采用QuEChERS前处理技术,超高效液相色谱-串联质谱电喷雾负离子模式检测测定。结果表明:在0... 建立了柑橘中虱螨脲、灭幼脲、氟啶脲和除虫脲4种苯甲酰脲类农药同时检测的超高效液相色谱-三重四级杆串联质谱( UPLC-MS/MS)分析方法。样品采用QuEChERS前处理技术,超高效液相色谱-串联质谱电喷雾负离子模式检测测定。结果表明:在0.01~0.2μg/mL范围内,4种供试农药的质量浓度与其相应的峰面积间呈良好的线性关系,相关系数( r )均大于0.994。在0.01、0.05和0.1 mg/kg 3个添加水平下,4种农药的平均回收率为92%~105%,相对标准偏差(RSD)为0.4%~3.3%(n=5)。4种农药在柑橘中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、简单,适用于同时测定柑橘中4种苯甲酰脲类农药的残留量。 展开更多
关键词 超高效液相色谱-三重四级杆串联质谱 柑橘 苯甲酰脲类农药 残留 ultra performance liquid chromatography-tandem mass spectrometry ( UPLC-MS/MS )
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超高效液相色谱-串联质谱法测定豇豆中溴氰虫酰胺等5种农药残留 被引量:17
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作者 钱程 吴琼 +1 位作者 吕岱竹 李建国 《农药学学报》 CAS CSCD 北大核心 2014年第5期594-599,共6页
建立了超高效液相色谱-串联质谱( UPLC-MS/MS)同时测定豇豆中溴氰虫酰胺、乙基多杀菌素、呋虫胺、噻虫嗪和啶虫脒残留量的方法。豇豆样品经乙腈提取,通过QuEChERS法净化后,采用Acquity UPLC?? BEH C18色谱柱分离,在电喷雾正离子... 建立了超高效液相色谱-串联质谱( UPLC-MS/MS)同时测定豇豆中溴氰虫酰胺、乙基多杀菌素、呋虫胺、噻虫嗪和啶虫脒残留量的方法。豇豆样品经乙腈提取,通过QuEChERS法净化后,采用Acquity UPLC?? BEH C18色谱柱分离,在电喷雾正离子模式下以多反应监测( MRM)模式检测。结果表明:在0.01~1μg/mL内5种农药的峰面积与其相应的质量浓度间呈良好线性关系,相关系数均大于0.99;在0.01、0.1和1 mg/kg 3个添加水平下,回收率为71%~129%,相对标准偏差为0.90%~20.8%( n =5)。5种农药在豇豆中的检出限为0.084~4.0μg/kg,定量限为0.80~16.6μg/kg。该方法简单灵敏,定量准确,可用于分析豇豆中的溴氰虫酰胺、乙基多杀菌素、呋虫胺、噻虫嗪和啶虫脒的残留量。 展开更多
关键词 超高效液相色谱-串联质谱 豇豆 溴氰虫酰胺 乙基多杀菌素 呋虫胺 噻虫嗪 啶虫脒 残留 ultra liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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超高效液相色谱-串联质谱双内标法同时测定复方杏香兔耳风胶囊中的10种有效成分 被引量:5
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作者 范晓苏 庞倩 徐远金 《色谱》 CAS CSCD 北大核心 2014年第3期216-223,共8页
建立了同时测定复方杏香兔耳风胶囊中原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III 和白术内酯 I 等10种有效成分含量的超高效液相色谱-串联质谱( UPLC-MS / MS)双内标分析方法。以咖... 建立了同时测定复方杏香兔耳风胶囊中原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III 和白术内酯 I 等10种有效成分含量的超高效液相色谱-串联质谱( UPLC-MS / MS)双内标分析方法。以咖啡酸和淫羊藿苷为内标(IS),在 ZORBAX RRHD Eclipse Plus C 18色谱柱上,以甲醇和含0.3%甲酸的水为流动相进行梯度洗脱分离,流速为0.3 mL / min。在电喷雾电离(ESI)正、负离子切换模式下,采用多重反应监测模式进行检测。结果表明,原儿茶酸、原儿茶醛、绿原酸、野黄芩苷、异绿原酸 C、黄芩苷、木犀草素、芹菜素、白术内酯 III、白术内酯 I 的线性范围分别为0.00300~24.0 mg / L、0.0170~2.00 mg / L、0.0150~30.0 mg / L、0.00400~30.0 mg / L、0.0105~24.0 mg / L、0.00300~30.0 mg / L、0.00300~5.00 mg / L、0.00600~5.00 mg / L、0.00150~4.00 mg / L、0.000600~0.900 mg / L;检出限分别为1.0、11、5.0、1.5、3.5、1.0、1.0、2.0、0.50、0.20μg / L。10种成分的加样回收率为92.5%~106%,相对标准偏差均不大于3.2%。该方法快速简便、灵敏度高、重复性好,已成功用于实际样品的分析。 展开更多
关键词 超高效液相色谱-串联质谱 有效成分 复方杏香兔耳风胶囊 ultra performance liquid chromatography-tandem mass spectrometry( UPLC-MS MS)
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高效液相色谱-串联质谱法测定水产品中甲氧苄啶的残留 被引量:6
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作者 万译文 李小玲 邓克国 《食品研究与开发》 CAS 北大核心 2014年第13期110-112,共3页
建立水产品中甲氧苄啶药物残留量测定的高效液相色谱-串联质谱方法。样品选择乙腈提取,用正己烷脱脂,固相萃取柱净化,采用LC-MS/MS选择反应监测(SRM)正离子模式测定进行定性、定量分析。结果表明:甲氧苄啶药物的检出限(LOD)为0.... 建立水产品中甲氧苄啶药物残留量测定的高效液相色谱-串联质谱方法。样品选择乙腈提取,用正己烷脱脂,固相萃取柱净化,采用LC-MS/MS选择反应监测(SRM)正离子模式测定进行定性、定量分析。结果表明:甲氧苄啶药物的检出限(LOD)为0.5μg/kg,定量限(LOQ)为1.0μg/kg,检测结果的相对标准偏差为1.78%-5.08%,加标回收率达到77.1%-93.5%。该方法具有比较高的重现性和选择性,在水产品中甲氧苄啶的残留测定中具有很好的应用前景。 展开更多
关键词 高效液相色谱-串联质谱法 内标法 甲氧苄啶 水产品 high performance liquid chromatography-tandem mass spectrometry (HPLC-MS MS)
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反相液相色谱-串联质谱法鉴定油菜蜂花粉中的蛋白质及活性肽 被引量:4
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作者 郭静 晏嘉泽 +1 位作者 郭明 靳艳 《色谱》 CAS CSCD 北大核心 2014年第3期284-289,共6页
基于鸟枪法蛋白质组学分析方法,使用反相液相色谱-串联质谱(RPLC-MS/MS)系统分析油菜蜂花粉蛋白质的胰蛋白酶酶解产物,结合数据库检索,共鉴定到353条肽段。鉴定到的肽段所归属的蛋白质中有239个蛋白质可检索到其分子生物学功能,主要功... 基于鸟枪法蛋白质组学分析方法,使用反相液相色谱-串联质谱(RPLC-MS/MS)系统分析油菜蜂花粉蛋白质的胰蛋白酶酶解产物,结合数据库检索,共鉴定到353条肽段。鉴定到的肽段所归属的蛋白质中有239个蛋白质可检索到其分子生物学功能,主要功能为结合活性、酶活性、运输活性、抑制活性等。根据血管紧张素转化酶(ACE)抑制肽活性与多肽构效之间的关系,从鉴定到的肽段中筛选并适当修饰后得到5条可能具有ACE抑制活性的肽段,化学合成肽段后进行了活性验证。结果表明5条肽段均具有良好的活性,其中肽段AELDIVLALF和LAVNLIPFP表现出较高的ACE抑制活性,半数抑制浓度(IC50)分别为(10.65±0.50)μmol/L和(23.66±1.08)μmol/L。该方法速度快,成本低,大大缩短了鉴定周期,达到了高通量筛选生物活性肽的目的。 展开更多
关键词 反相液相色谱-串联质谱 蛋白质 血管紧张素转化酶抑制肽 油菜蜂花粉 REVERSED-PHASE liquid chromatography-tandem mass spectrometry ( RPLC-MS MS)
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液相色谱-四极杆飞行时间质谱法筛查猪肉中5类26种药物残留 被引量:7
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作者 谢寒冰 王毅刚 +4 位作者 周明莹 赵海峰 蒋万枫 邓书 董诗竹 《分析测试学报》 CAS CSCD 北大核心 2014年第4期373-379,共7页
建立了同时筛查测定猪肉组织中氟喹诺酮类、磺胺类、有机磷类、β-激动剂类、四环素类5类26种药物残留的液相色谱-四极杆飞行时间质谱分析方法.试样采用QuEChERS前处理方法,样品经酸化乙腈-甲醇(1%乙酸,10%甲醇)提取.提取液以C18分... 建立了同时筛查测定猪肉组织中氟喹诺酮类、磺胺类、有机磷类、β-激动剂类、四环素类5类26种药物残留的液相色谱-四极杆飞行时间质谱分析方法.试样采用QuEChERS前处理方法,样品经酸化乙腈-甲醇(1%乙酸,10%甲醇)提取.提取液以C18分散剂和正己烷净化,氮吹浓缩、定容后过滤膜上机检测.液相色谱以甲醇-水(0.1%甲酸)作为流动相梯度洗脱,C18色谱柱分离;高分辨质谱采用正离子模式检测,以二级质谱特征离子定性,以分子离子精确质量数提取色谱峰面积定量.结果表明26种药物的定量下限为0.4~10μg/kg;加标回收率为56.7%~106.2%,相对标准偏差(RSD)为7.7%~15.8%.方法操作简单、快速、高效,可作为猪肉中26种药物残留的快速筛查检测方法. 展开更多
关键词 液相色谱-四极杆飞行时间质谱 猪肉 兽药 多残留 快速筛查 high performance liquid chromatography-tandem mass spectrometry(HPLC-Q-TOF-MS)
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高效液相色谱-串联质谱法测定食品添加剂中蛇床子素含量
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作者 李昱 吴胜明 +3 位作者 方均建 马昆鹏 宋占军 董方霆 《分析测试学报》 CAS CSCD 北大核心 2007年第z1期242-243,247,共3页
To establish HPLC electrospray ionization mass spectrometry (HPLC-ESI MS) method for determination of osthole in food additive.The samples were dipped in methanol overnight and extracted with it by ultrasonic instrume... To establish HPLC electrospray ionization mass spectrometry (HPLC-ESI MS) method for determination of osthole in food additive.The samples were dipped in methanol overnight and extracted with it by ultrasonic instrument,then the supernatant was send to sampler for detection.Sample was chromatographed using 0.4%HAc solution-MeOH (35:65,by volume) mobile phase on an Xterra MS C18 column.Analyte determination was performed by ESI MS/MS in the multiple reaction monitoring(MRM)mode.The established method of LC-MS/MS determining the concentration of osthole in food additive has the characteristic of strong specificity,high sensitivity and good reproducibility.The linear range of papaverine was 0.001-10 μg/mL,method recovery was 97.42%,RSD was 8.37%,the limit of detection was 1 ng/mL and the limit of quantitation was 0.001 μg/mL. 展开更多
关键词 OSTHOLE Liquid chromatography-tandem mass spectrometry(LC-MS/MS)
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液相色谱-串联质谱法测定中药材中11种真菌毒素 被引量:4
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作者 刘静 朱叶梅 +5 位作者 董胜强 杨盼盼 廖予琦 杨飚 张建 李瑞 《化学分析计量》 CAS 2022年第10期15-20,共6页
建立液相色谱-串联质谱(LC-MS/MS)法同时测定中药材中11种真菌毒素的方法。样品经乙腈-水提取,以0.1%甲酸甲醇溶液-0.1%甲酸水溶液为流动相,用Waters Acquity BEH C柱分离,采用LC-MS/MS法测定,内标法定量。11种真菌毒素的质量浓度在0.1~... 建立液相色谱-串联质谱(LC-MS/MS)法同时测定中药材中11种真菌毒素的方法。样品经乙腈-水提取,以0.1%甲酸甲醇溶液-0.1%甲酸水溶液为流动相,用Waters Acquity BEH C柱分离,采用LC-MS/MS法测定,内标法定量。11种真菌毒素的质量浓度在0.1~100 ng/mL范围内线性关系良好,相关系数均不小于0.996,检出限为0.08~1.40μg/kg。样品加标回收率为76.1%~97.6%,测定结果的相对标准偏差为3.97%~8.58%(n=6)。该方法简单、稳定、可靠,适合中药材中11种真菌毒素的测定。 展开更多
关键词 中药材 液相色谱-串联质谱法 真菌毒素
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Pharmacokinetics and bioavailability of R-phencynonate in Beagle dogs
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作者 LI Jing-lai,CUI Meng-cun,WANG Xiao-ying,QIAO Jian-zhong,ZHANG Zhen-qing,RUAN Jin-xiu,ZhONG Bo-hua,LIU Ke-liang(Beijing Institute of Pharmacology and Toxicology,Beijing 100850,China) 《沈阳药科大学学报》 CAS CSCD 北大核心 2008年第S1期98-98,共1页
Objective To evaluate the pharmacokinetics(PK)properties and bioavailability of R-phencynonate(L-8021)in Beagle dogs.Methods Fifteen healthy Beagle dogs were randomly divided into three groups,each group was orally gi... Objective To evaluate the pharmacokinetics(PK)properties and bioavailability of R-phencynonate(L-8021)in Beagle dogs.Methods Fifteen healthy Beagle dogs were randomly divided into three groups,each group was orally given single dose of 0.1 mg·kg-1,0.4 mg·kg-1 and 1.2 mg·kg-1 R-phencynonate respectively.After one week cleaning,the middle dose group was injected 0.4 mg·kg-1 dose.Blood samples(about 2 mL)were collected in heparinized tubes before dosing and at 0.033,0.083,0.25,0.5,0.75,1,2,4,6,8,12 h after administration,and were then immediately centrifuged at 2000 g for 15 min.The pharmacokinetics(PK)properties and bioavailability of the drugs was evaluated using the liquid chromatographic-tandem mass spectrometric(LC-MS/MS)method.Results After p.o.administration of 0.1,0.4 and 1.2 mg·kg-1 R-phencynonate,tmax ranged within 0.65-1.2 h;t1/2z ranged within 2.84-3.36 h;CLz/F ranged within 5.00-9.32 L·h-1·kg-1;Cmax ranged within 1.87-70.34 ng·mL-1;AUC(0-t)ranged within 9.80-250.12 μg·L-1·h;After i.v.administration of 0.4 mg·kg-1,t1/2z was 2.52 h;AUC(0-t)was 238.11 μg·L-1·h.Conclusions L-8021 was dose-dependent within the range of 0.1-1.2 mg·kg-1 in Beagle dogs and the blood drug concentration-time curves were all best fitted to first order absorption two-compartment open model after via po administration of three different dosages.Following oral administration to Beagle dogs,the absolute bioavailability of L-8021 was 17.82%,which was very low and resulted from poor absorption. 展开更多
关键词 R-phencynonate liquid chromatography-tandem ELECTROSPRAY mass spectrometry
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Ribotrap Analysis of Proteins Associated with FHL3 3'Untranslated Region in Glioma Cells
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作者 Wei Han Qing Xia +1 位作者 Bin Yin Xiao-zhong Peng 《Chinese Medical Sciences Journal》 CAS CSCD 2014年第2期78-84,共7页
Objective To screen the proteins associated with four-and-a-half LIM domains 3(FHL3) 3' untranslated region(3'UTR) in glioma cells. Methods Western blot was adopted to detect the regulatory effect of poly(C)-b... Objective To screen the proteins associated with four-and-a-half LIM domains 3(FHL3) 3' untranslated region(3'UTR) in glioma cells. Methods Western blot was adopted to detect the regulatory effect of poly(C)-binding protein 2(PCBP2) on FHL3. Biotin pull-down and sliver staining were employed to screen and verify the candidate binding proteins of FHL3 3'UTR. Then liquid chromatography-tandem mass spectrometry(LC-MS/MS) and molecule annotation system were used to identify and analyze the candidate binding proteins. Immunoprecipitation was conducted to study the interaction between PCBP2 and polypyrimidine tract-binding protein 1(PTBP1), a binding protein identified by LC-MS/MS. Results PCBP2 could bind to FHL3 mRNA 3'UTR-A and inhibited the expression of FHL3 in T98 G glioms cells. 22 candidate binding proteins were identified. Among them, there were 11 RNA binding proteins, including PCBP2. PTBP1 associated with FHL3 mRNA 3'UTR and interacted with PCBP2 protein. Conclusion PCBP2 and PTBP1 can both associate with FHL3 mRNA 3'UTR through forming a protein complex. 展开更多
关键词 FHL3 3'untranslated region poly(C)-binding protein 2 polypyrimidine tract-binding protein 1 liquid chromatography-tandem mass spectrometry
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