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Determination of Benzo[a]pyrene in Edible Oil by High Performance Liquid Chromatography-Fluorescence Detector (HPLC-FL)
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作者 Guixia YANG Jie LIU +3 位作者 Xiujuan WANG Fenglan ZHANG Kun XIN Chunli KONG 《Agricultural Biotechnology》 2024年第2期8-9,19,共3页
In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Sc... In this study, an optimized high performance liquid chromatography-fluorescence detector (HPLC-FL) method for the determination of benzo[a]pyrene in edible oil was established. HPLC was performed with Thermo Fisher Scientific C18 column (250 mm×4.6 mm, 5 μm) as the chromatographic column and acetonitrile and water as the mobile phase, and the excitation wavelength and emission wavelength of fluorescence detector were 286 and 430 nm, respectively. The response was high, and the linear range was 0.5-10.0 ng/ml. The lowest limit of detection was 0.11 ng/ml, and the average recovery was 92.5%. This method is suitable for quantitative analysis of benzo[a]pyrene content in edible oil. 展开更多
关键词 BENZO[A]PYRENE High performance liquid chromatography Fluorescence detector
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High throughput and rapid isolation of extracellular vesicles and exosomes with purity using size exclusion liquid chromatography
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作者 Kshipra S.Kapoor Kristen Harris +5 位作者 Kent A.Arian Lihua Ma Beatriz Schueng Zancanela Kaira A.Church Kathleen M.McAndrews Raghu Kalluri 《Bioactive Materials》 SCIE CSCD 2024年第10期683-695,共13页
Extracellular vesicles(EVs)have emerged as potential biomarkers for diagnosing a range of diseases without invasive procedures.Extracellular vesicles also offer advantages compared to synthetic vesicles for delivery o... Extracellular vesicles(EVs)have emerged as potential biomarkers for diagnosing a range of diseases without invasive procedures.Extracellular vesicles also offer advantages compared to synthetic vesicles for delivery of various drugs;however,limitations in segregating EVs from other particles and soluble proteins have led to inconsistent EV retrieval rates with low levels of purity.Here,we report a new high-yield(88.47%)and rapid(<20 min)EV isolation method termed size exclusion–fast protein liquid chromatography(SE-FPLC).We show SE-FPLC can effectively isolate EVs from multiple sources including EVs derived from human and mouse cells and serum samples.The results indicate that SE-FPLC can successfully remove highly abundant protein contaminants such as albumin and lipoprotein complexes,which can represent a major hurdle in large scale isolation of EVs.The high-yield nature of SE-FPLC allows for easy industrial scaling up of EV production for various clinical utilities.SE-FPLC also enables analysis of small volumes of blood for use in point-of-care diagnostics in the clinic.Collectively,SE-FPLC offers many advantages over current EV isolation methods and offers rapid clinical translation. 展开更多
关键词 Extracellular vesicles Size exclusion-fast performance liquid chromatography Isolation methods
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HPLC及LC-MS测定榛子中氯吡苯脲和多菌灵残留 被引量:1
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作者 桑育黎 王沛 +2 位作者 郝延军 李楠楠 戚建忠 《辽宁大学学报(自然科学版)》 CAS 2024年第1期8-15,共8页
本文采用高效液相色谱法(HPLC)和液相色谱-质谱法(LC-MS)对干果榛子中氯吡苯脲和多菌灵残留量进行含量测定.HPLC和LC-MS均使用C18色谱柱,含量测定采取等度洗脱,流动相:甲醇-水(55∶45,体积比);体积流量:1.0 mL·min-1;测定波长:260 ... 本文采用高效液相色谱法(HPLC)和液相色谱-质谱法(LC-MS)对干果榛子中氯吡苯脲和多菌灵残留量进行含量测定.HPLC和LC-MS均使用C18色谱柱,含量测定采取等度洗脱,流动相:甲醇-水(55∶45,体积比);体积流量:1.0 mL·min-1;测定波长:260 nm;柱温:30℃.LC-MS采取电喷雾离子源,梯度洗脱,体积流量:0.6 mL·min-1,柱温:30℃.结果表明,榛子中氯吡苯脲与多菌灵存在残留,氯吡苯脲质量浓度在1.00~10.00μg·mL-1范围内线性关系良好,加样回收率在95.58%~100.58%;多菌灵质量浓度在1.005~15.075μg·mL-1范围内具有良好的线性关系,加样回收率在95.61%~104.39%.实验证明,HPLC与LC-MS相结合的方法具有操作简便、灵敏度高、检出限低等优点,能有效地检测到榛子样品中膨大剂氯吡苯脲及杀菌剂多菌灵的残留,并确定其残留量,线性关系和回收率结果均令人满意.根据被检测的8批样品中氯吡苯脲和多菌灵两项农药残留量推断,作为一般干果食用榛子是安全的. 展开更多
关键词 榛子 氯吡苯脲 多菌灵 高效液相色谱法(hplc) 液相色谱-质谱法(LC-MS)
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基于HPLC法及UPLC-MS法测定芫花饮片炮制前后7种成分的含量变化
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作者 张萍 米宏英 +4 位作者 严华 魏锋 高慧媛 马双成 陆兔林 《中国药事》 CAS 2024年第5期575-587,共13页
目的:建立HPLC法及UPLC-MS法测定芫花中银椴苷、木犀草素、芹菜素、绿原酸、羟基芫花素、芫花素及芫花酯甲7种化学成分含量的方法,分析芫花炮制前后化学成分的变化。方法:采用HPLC法,测定银椴苷、木犀草素、芹菜素、绿原酸、羟基芫花素... 目的:建立HPLC法及UPLC-MS法测定芫花中银椴苷、木犀草素、芹菜素、绿原酸、羟基芫花素、芫花素及芫花酯甲7种化学成分含量的方法,分析芫花炮制前后化学成分的变化。方法:采用HPLC法,测定银椴苷、木犀草素、芹菜素、绿原酸、羟基芫花素和芫花素6种成分的含量,色谱柱为Agilent Eclipse Plus C18(250 mm×4.6 mm,5μm),流动相为乙腈(A)-0.1%甲酸(B)梯度洗脱,流速为1.0 mL·min^(-1),进样量10μL。同时采用UPLC-MS方法测定芫花酯甲的含量,色谱柱为ACQUITY UPLC HSS T3 C18色谱柱(2.1 mm×100 mm,1.8μm),流动相为乙腈(A)-0.1%甲酸(B)梯度洗脱,流速0.3 mL·min-1,柱温35℃,进样量1μL。结果:7种成分的含量由高到低依次为芫花素>绿原酸>银椴苷>芹菜素>羟基芫花素>木犀草素>芫花酯甲。芫花炮制后7种成分的含量均发生一定程度的变化,其中绿原酸成分在炮制后含量有升高有降低,变化不明显;对于银椴苷和芹菜素成分,炮制后含量降低;对于木犀草素、羟基芫花素和芫花素3个成分,炮制后含量升高;对于芫花酯甲成分,炮制后含量降低。结论:该方法简便、灵敏、高效,为考察芫花饮片炮制前后的质量变化提供了技术支持。 展开更多
关键词 芫花 炮制 化学成分 含量测定 液相色谱 液质联用色谱
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基于UHPLC-Q-Exactive Orbitrap HRMS技术结合化学计量学方法的不同干燥处理杜仲叶成分分析 被引量:1
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作者 李淑芳 王会锋 +6 位作者 郝学飞 胡永建 李圆圆 马风莲 冯书惠 杨亚琴 于永杰 《分析测试学报》 CAS CSCD 北大核心 2024年第2期213-225,共13页
采用基于液质联用的非靶向代谢组学技术结合化学计量学数据自动解析软件AntDAS-LCHRMS分析了4种不同干燥处理(冻干、热泵烘干、电热烘干、晒干)杜仲叶样本中的化合物。杜仲叶样本数据由超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UH... 采用基于液质联用的非靶向代谢组学技术结合化学计量学数据自动解析软件AntDAS-LCHRMS分析了4种不同干燥处理(冻干、热泵烘干、电热烘干、晒干)杜仲叶样本中的化合物。杜仲叶样本数据由超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(UHPLC-Q-Exactive Orbitrap HRMS)分别在正、负离子模式下进行采集,经AntDAS-LCHRMS软件解析,共鉴定出71种差异性化合物,经标准品验证确定40种化合物,包括环烯醚萜类、有机酸类、黄酮类、氨基酸类、核苷类、维生素类等9类物质。其中,正、负离子模式下均可识别并验证的化合物有车叶草苷、绿原酸、芦丁、异槲皮苷、车叶草苷酸、京尼平苷等25种化合物。层次聚类分析(HCA)及主成分分析(PCA)结果均显示,相同处理的杜仲叶样本各自聚成一类,不同处理的杜仲叶样本可明显区分。热图分析进一步揭示了不同干燥处理杜仲叶样本中差异性化合物的含量变化。晒干处理样本中苯丙氨酸及色氨酸等氨基酸类物质的水平较高;冻干及热泵烘干处理样本中有机酸类、环烯醚萜类、糖类等含量较高;电热烘干样本中核苷类、黄酮类物质的含量较高;黄酮类物质在冻干、热泵烘干及晒干样本中差异较小。研究结果为不同干燥处理杜仲叶的成分分析、品质评价及其开发应用提供了科学依据,也可为其他复杂药用植物体系的化学成分分析提供参考。 展开更多
关键词 杜仲叶 代谢组学 化学计量学 AntDAS-LCHRMS软件 超高效液相色谱-四极杆-静电场轨道阱高分辨质谱(Uhplc-Q-Exactive Orbitrap HRMS) 干燥处理
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基于高效液相色谱(HPLC)的微生物发酵过程中的关键代谢物分析 被引量:1
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作者 吴世芳 《工业微生物》 CAS 2024年第1期197-199,共3页
微生物发酵是生物工程和工业生物技术的核心过程,涉及多种复杂的生物化学变化,其发酵过程中产生的代谢物对于理解微生物的生理状态和优化生产过程至关重要。高效液相色谱(HPLC)作为一种高效、精确的分析方法,在识别和定量这些代谢物方... 微生物发酵是生物工程和工业生物技术的核心过程,涉及多种复杂的生物化学变化,其发酵过程中产生的代谢物对于理解微生物的生理状态和优化生产过程至关重要。高效液相色谱(HPLC)作为一种高效、精确的分析方法,在识别和定量这些代谢物方面发挥着关键作用。文章基于高效液相色谱(HPLC)对微生物发酵过程中的关键代谢物展开分析,以期为微生物发酵过程的控制和优化提供参考。 展开更多
关键词 高效液相色谱 微生物发酵 关键代谢物
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HPLC法测定十三味逐瘀合剂中游离大黄酚含量
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作者 邓凤云 王建芳 +3 位作者 吴显兴 韦贤 罗试计 姜攀 《右江医学》 2024年第1期51-56,共6页
目的建立十三味逐瘀合剂中大黄酚高效液相含量测定的方法。方法采用高效液相色谱法(HPLC法)对十三味逐瘀合剂中游离大黄酚含量进行测定,从提取溶剂、取样量、提取时间等影响因素中选出最优条件,建立完整的含量测定方法。结果用thermos ... 目的建立十三味逐瘀合剂中大黄酚高效液相含量测定的方法。方法采用高效液相色谱法(HPLC法)对十三味逐瘀合剂中游离大黄酚含量进行测定,从提取溶剂、取样量、提取时间等影响因素中选出最优条件,建立完整的含量测定方法。结果用thermos C18色谱柱(250 mm×4.6 mm,5μm);以甲醇-0.1%磷酸(75∶25,V/V)为流动相,采用等度洗脱法,254 nm波长的色谱条件;以甲醇为浸膏提取溶剂,超声30 min的提取方法;大黄酚质量浓度在1.63~16.32μg/mL(R^(2)=0.9995)范围内具有良好的线性关系;平均回收率为104.17%;测得十三味逐瘀合剂中游离大黄酚平均含量为15.32μg/mL。结论本实验所建立的方法操作简单,专属性强,重现性好,可用于十三味逐瘀合剂中游离大黄酚的含量测定。 展开更多
关键词 十三味逐瘀合剂 含量 大黄酚 高效液相色谱法
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HPLC-ELSD同时测定腺梗豨莶草中6个二萜成分的含量
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作者 殷玥 张璇 呼小娜 《中国兽医杂志》 CAS 北大核心 2024年第1期144-150,共7页
为了研究腺梗豨莶草中6个二萜成分(对映海松烯型二萜:奇任醇、Hythiemoside B和豨莶精醇;对映贝壳杉烷型二萜:对映-17,18-二羟基-贝壳杉烷-19-羧酸、对映-16β,17-二羟基-贝壳杉烷-19-羧酸和对映-16α氢-贝壳杉烷-17,19-二羧酸)的含量,... 为了研究腺梗豨莶草中6个二萜成分(对映海松烯型二萜:奇任醇、Hythiemoside B和豨莶精醇;对映贝壳杉烷型二萜:对映-17,18-二羟基-贝壳杉烷-19-羧酸、对映-16β,17-二羟基-贝壳杉烷-19-羧酸和对映-16α氢-贝壳杉烷-17,19-二羧酸)的含量,本试验建立了高效液相色谱法-蒸发光散射检测器(HPLC-ELSD)同时测定二萜类化合物含量。样品粉碎过筛加甲醇和乙酸乙酯回流提取,蒸发减压除去溶剂,甲醇溶解,0.45μm滤膜滤过,取续滤液进行测定。色谱条件:色谱柱为Waters Symmetry Shield^(TM)RP18柱(250 mm×4.6 mm,5μm),流动相为0.3%甲酸水溶液-乙腈(v/v),梯度洗脱,流速为1.0 mL/min。蒸发光散射检测器漂移管温度为103℃,雾化气流速为3.0 L/min。应用该方法测定腺梗豨莶草样品不同部位中6个二萜类化合物的含量,同时比较叶、枝、茎中对映海松烯型二萜、对映贝壳杉型二萜和总二萜含量的差异。结果显示,6个二萜成分在其线性范围内线性关系良好(r≥0.9992);日内和日间精密度相对标准偏差(RSD)均小于3.5%;回收率介于96.5%~101.5%,RSD均小于2.3%;腺梗豨莶草不同部位(叶、枝、茎)的二萜类化合物含量差异较大。结果表明,本试验所建立的HPLC-ELSD方法简便、准确、重复性好,为腺梗豨莶草药材全面的质量评价和临床应用中最佳药用部位的选择提供了参考。 展开更多
关键词 高效液相色谱法(hplc) 蒸发光散射检测器(ELSD) 腺梗豨莶草 含量测定 质量控制
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HPLC法测定兰柏消炎膏中盐酸小檗碱的含量
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作者 陈燕梨 梁诗敏 +3 位作者 刁军飞 杨贤娜 柴莉娜 李卓亚 《广东化工》 CAS 2024年第2期121-123,共3页
目的:制备以黄柏为君药的兰柏消炎方的软膏剂,经过高效液相色谱法测定君药黄柏中的盐酸小檗碱的含量,为该制剂的工业化生产与质量控制提供参考。方法:以黄柏、侧柏叶、大黄、薄荷、泽兰等为主药制备兰柏消炎膏,采用高效液相色谱法测定... 目的:制备以黄柏为君药的兰柏消炎方的软膏剂,经过高效液相色谱法测定君药黄柏中的盐酸小檗碱的含量,为该制剂的工业化生产与质量控制提供参考。方法:以黄柏、侧柏叶、大黄、薄荷、泽兰等为主药制备兰柏消炎膏,采用高效液相色谱法测定其盐酸小檗碱的含量,以45∶55的比例将乙腈与0.1%的磷酸溶液混合,作为流动相溶液,其中每100 mL的流动相溶液中需要添加0.1 g的十二烷基磺酸钠。以1.0 mL·min^(-1)的流速操作,每次的采集量设定为10μL,并且所采集的光谱范围是265 nm,柱温为25℃的色谱条件下检测对兰柏消炎膏中的盐酸小檗碱进行测定,并进行方法学考察。结果:在该色谱条件下,溶剂和阴性溶液对盐酸小檗碱的测定无吸收峰的干扰。盐酸小檗碱的峰面积在11.8~141.6μg·mL^(-1)的浓度范围内呈现出上升趋势,其回归方程Y=38905X-65.441,R^(2)=0.9957,这表明盐酸小檗碱的峰面积与其浓度之间存在着良好的线性关联。结论:建立的盐酸小檗碱含量测定方法简便合理、准确,稳定可行,可用于兰柏消炎膏的质量控制。 展开更多
关键词 兰柏消炎膏 小檗碱 质量控制 高效液相色谱法
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HPLC-MS/MS法同时测定胆木不同部位6个成分的含量
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作者 贾安 黄小强 +3 位作者 茹国华 吴毓皇 明古旭 李永辉 《中药材》 CAS 北大核心 2024年第2期398-402,共5页
目的:测定胆木茎、枝和叶中异长春花苷内酰胺、喜果苷、乌檀酰胺C、绿原酸、3,4,5-三甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷、3,4-二甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷6个成分的含量。方法:采用HPL... 目的:测定胆木茎、枝和叶中异长春花苷内酰胺、喜果苷、乌檀酰胺C、绿原酸、3,4,5-三甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷、3,4-二甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷6个成分的含量。方法:采用HPLC-MS/MS法,色谱柱为Phenomenex Kinete EVO C18100Å(50 mm×2.1 mm,2.6μm)柱;流动相为0.5‰甲酸溶液-甲醇,梯度洗脱;流速为0.4 mL/min;柱温为40℃;进样量为3μL;电喷雾离子源,多反应监测负离子模式。结果:异长春花苷内酰胺、喜果苷、乌檀酰胺C、绿原酸、3,4,5-三甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷、3,4-二甲氧基苯基-1-O-β-呋喃芹糖基(1→2)-β-D-吡喃葡萄糖苷的线性范围分别为0.025~2μg/mL、0.0125~2μg/mL、0.05~2μg/mL、0.025~2μg/mL、0.0125~2μg/mL、0.0125~2μg/mL(r≥0.9991),精密度、稳定性(24 h)、重复性试验RSD<5.00%,平均加样回收率为95.13%~103.02%(RSD<4.00%)。含量测定结果显示6个成分在胆木不同部位中的含量存在较大差异。结论:所建立的方法简便、快速、灵敏,适用于胆木药材中6个成分的同时检测。 展开更多
关键词 胆木 化学成分 含量测定 高效液相色谱-串联质谱法
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Efficient and selective extraction of uranium from seawater based on a novel pulsed liquid chromatography radionuclide separation method 被引量:2
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作者 Jian‑Hua Ye Tao Yu 《Nuclear Science and Techniques》 SCIE EI CAS CSCD 2023年第2期13-27,共15页
The novel pulsed liquid chromatography radionuclide separation method presented here provides a new and promising strategy for the extraction of uranium from seawater.In this study,a new chromatographic separation met... The novel pulsed liquid chromatography radionuclide separation method presented here provides a new and promising strategy for the extraction of uranium from seawater.In this study,a new chromatographic separation method was proposed,and a pulsed nuclide automated separation device was developed,alongside a new chromatographic column.The length of this chromatographic column was 10 m,with an internal warp of 3 mm and a packing size of 1 mm,while the total separation units of the column reached 12,250.The most favorable conditions for the separation of nuclides were then obtained through optimizing the separation conditions of the device:Sample pH in the column=2,sample injection flow rate=5.698 mL/min,chromatographic column heating temperature=60℃.Separation experiments were also carried out for uranium,europium,and sodium ions in mixed solutions;uranium and sodium ions in water samples from the Ganjiang River;and uranium,sodium,and magnesium ions from seawater samples.The separation factors between the different nuclei were then calculated based on the experimental data,and a formula for the separation level was derived.The experimental results showed that the separation factor in the mixed solution of uranium and europium(1:1)was 1.088,while achieving the initial separation of uranium and europium theoretically required a 47-stage separation.Considering the separation factor of 1.50for the uranium and sodium ions in water samples from the Ganjiang River,achieving the initial separation of uranium and sodium ions would have theoretically required at least a 21-stage separation.Furthermore,for the seawater sample separation experiments,the separation factor of uranium and sodium ions was 1.2885;therefore,more than 28 stages of sample separation would be required to achieve uranium extraction from seawater.The novel pulsed liquid chromatography method proposed in this study was innovative in terms of uranium separation and enrichment,while expanding the possibilities of extracting uranium from seawater through chromatography. 展开更多
关键词 Pulsed liquid chromatography Nuclide separation Seawater uranium extraction Uranium enrichment
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基于UHPLC-QTOF-MS的兰州百合植物化学成分鉴定 被引量:2
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作者 米璐 王珂雯 +4 位作者 祝秀梅 王雪 杨曙明 廖小军 徐贞贞 《食品工业科技》 CAS 北大核心 2024年第2期48-58,共11页
为探究地理标志产品兰州百合(Lilium davidii var.unicolor)的植物化学成分,以甘肃省五个主要产区(兰州市榆中县、兰州市七里河区、定西市临洮县、定西市渭源县、临夏市永靖县)的兰州百合鳞茎为研究对象,基于超高效液相色谱串联四极杆... 为探究地理标志产品兰州百合(Lilium davidii var.unicolor)的植物化学成分,以甘肃省五个主要产区(兰州市榆中县、兰州市七里河区、定西市临洮县、定西市渭源县、临夏市永靖县)的兰州百合鳞茎为研究对象,基于超高效液相色谱串联四极杆飞行时间质谱法的非靶向代谢组学技术鉴定其植物化学成分。结果表明,在兰州百合鳞茎中初步鉴定出62种植物化学成分,包含谷胱甘肽等22种氨基酸、多肽及其衍生物,溶血磷脂酰胆碱等9种油脂和磷脂类,鼠李糖等7种糖类,阿魏酸、咖啡酸等7种酚酸类,山奈酚等4种黄酮类,核黄素、维生素C等4种天然维生素,阿魏酰腐胺等3种酚胺类,大丁苷等2种香豆素类,葫芦巴碱等2种生物碱,萜类组分松香酸和三萜皂苷类组分刺五加苷E。本研究丰富了兰州百合植物化学成分的现有数据,为兰州百合的研究与利用提供了科学依据。 展开更多
关键词 兰州百合 植物化学成分 代谢组学 超高效液相色谱串联四极杆飞行时间质谱法(Uhplc-QTOF MS) R语言
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Determination of 5-Fluorouracil in Human Plasma by High-Performance Liquid Chromatography (HPLC) 被引量:2
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作者 谷元 陆榕 +1 位作者 司端运 刘昌孝 《Transactions of Tianjin University》 EI CAS 2010年第3期167-173,共7页
5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its nar... 5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its narrow therapeutic index. Therefore, a simple, economic and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the determination of 5-FU in human plasma. Ethyl acetate was chosen as extraction reagent. Chromatographic separation was performed on a Diamonsil C18 column (250 mm × 4.6 mm i.d., 5 μm) with the mobile phase consisting of methanol and 20 mmol/L ammonium formate using a linear gradient elution at a flow rate of 0.8 mL/min. 5-FU and 5-bromouracil (5-BU) were detected by UV detector at 265 nm. The calibration curve was linear over the concentration range of 5—500 ng/mL and the correlation coefficient was not less than 0.992 6 for all calibration curves. The intra- and inter-day precisions were less than 10.5% and 4.3%, respectively, and the accuracy was within ±3.7%. The recovery at all concentration levels was 80.1±8.6%. 5-FU was stable under possible conditions of storing and handling. This method is proved applicable to therapeutic drug monitoring and pharmacokinetic studies of 5-FU in human. 展开更多
关键词 5-fluorouracil (5-FU) high-performance liquid chromatography (hplc human plasma
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小儿热速清口服液HPLC指纹图谱的建立及多指标成分的含量测定 被引量:1
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作者 崔俊凤 崔帅 +3 位作者 梁秀坤 李东旭 王鑫瑞 高鹏 《中国药房》 CAS 北大核心 2024年第7期801-806,共6页
目的建立小儿热速清口服液高效液相色谱(HPLC)指纹图谱,并对其中12种指标成分进行含量测定。方法采用HPLC法。以Venusil MP C18为色谱柱;以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱;流速为1.0 mL/min;检测波长为210 nm;柱温为30℃;进样量... 目的建立小儿热速清口服液高效液相色谱(HPLC)指纹图谱,并对其中12种指标成分进行含量测定。方法采用HPLC法。以Venusil MP C18为色谱柱;以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱;流速为1.0 mL/min;检测波长为210 nm;柱温为30℃;进样量为10μL。采用《中药色谱指纹图谱相似度评价系统(2012版)》建立13批小儿热速清口服液的HPLC指纹图谱,并进行相似度评价,测定12种指标成分,即(R,S)告依春、3,5-二-O-咖啡酰奎宁酸、葛根素、连翘苷、连翘酯苷A、绿原酸、黄芩苷、柴胡皂苷d、汉黄芩苷、黄芩素、大黄素、大黄酚的含量。结果13批小儿热速清口服液指纹图谱的相似度均大于0.97,指认了14个共有峰。13批小儿热速清口服液中上述12种指标成分的含量分别为0.078~0.172、1.564~2.736、1.338~2.578、0.426~0.872、1.477~2.628、1.396~2.447、4.052~9.146、0.367~0.692、1.974~4.674、1.274~2.969、0.085~0.167、0.155~0.307 mg/mL。结论本研究建立的HPLC指纹图谱及含量测定方法准确度高、专属性好,可用于小儿热速清口服液的质量评价。 展开更多
关键词 小儿热速清口服液 高效液相色谱法 指纹图谱 含量测定
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消瘀泄浊饮中活性成分鉴定以及HPLC法测定其中5种关键成分 被引量:1
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作者 范桢亮 鲁科达 +3 位作者 范军芬 张培培 夏虹 马红珍 《辽宁中医药大学学报》 CAS 2024年第5期32-37,共6页
目的利用高效液相色谱联合质谱技术鉴定消瘀泄浊饮中的活性成分,并利用HPLC法测定毛蕊异黄酮葡萄糖苷、大黄素、芦荟大黄素、杯苋甾酮、苦杏仁苷这5种成分的含量。方法采用液质联用技术测定消瘀泄浊饮中的生物活性成分,色谱柱:Waters HS... 目的利用高效液相色谱联合质谱技术鉴定消瘀泄浊饮中的活性成分,并利用HPLC法测定毛蕊异黄酮葡萄糖苷、大黄素、芦荟大黄素、杯苋甾酮、苦杏仁苷这5种成分的含量。方法采用液质联用技术测定消瘀泄浊饮中的生物活性成分,色谱柱:Waters HSS T3(100 mm×2.1 mm,1.8μm),流动相为0.1%甲酸-水溶液→0.1%甲酸-乙腈-异丙醇,梯度洗脱;流速:0.3 mL/min;柱温:40℃。高分辨质谱:鞘气40 Arb;辅助气10 Arb;离子喷雾电压3000 V/-2800 V;温度350℃;离子传输管温度320℃;扫描模式为Full-scan MS2模式。采用Progenesis QI进行基线过滤、峰识别、积分、保留时间校正、峰对齐,对比公共数据库和实验室自建数据库后得到消瘀泄浊饮中的生物活性成分。选择Sharpsil-U C_(18)色谱柱;流动相为甲醇→超纯水;梯度洗脱;流速:1.0 mL/min;柱温:30℃;进样量:10μL;检测波长:210 nm(苦杏仁苷、杯苋甾酮),260 nm(毛蕊异黄酮葡萄糖苷、大黄素、芦荟大黄素)。结果从消瘀泄浊饮中共找到276种生物活性成分,其中负离子模式下找到119种,正离子模式下找到157种。选择毛蕊异黄酮葡萄糖苷、大黄素、芦荟大黄素、杯苋甾酮、苦杏仁苷为消瘀泄浊饮的指标成分。各成分均能有效检出,分离度良好,阴性无干扰;5种成分在测定的进样浓度范围内与峰面积线性关系良好;平均加样回收率为99.94%~101.07%;RSD为0.78%~2.27%。结论液质联用技术可以有效鉴定消瘀泄浊饮中的生物活性成分,所建立的HPLC法稳定性好,特异性强,可以为消瘀泄浊饮的质量控制和评价提供参考依据。 展开更多
关键词 消瘀泄浊饮 高效液相色谱 高分辨质谱 成分鉴定 含量测定
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Determination of Organic Acids in Root Exudates by High Performance Liquid Chromatography: I. Development and Assessment of Chromatographic Conditions *1 被引量:4
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作者 SHENJIANBO ZHANGFUSUO 《Pedosphere》 SCIE CAS CSCD 1998年第2期97-104,共8页
Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile ph... Methods for determining nine low molecular weight organic acids in root exudates were developed by using reversed phase high performance liquid chromatography with UV (ultraviolet) detection at 214 nm. The mobile phase was 18 mmol L -1 kH 2PO 4 adjusted to pH 2.25 with phosphoric acid and the flow rate was 0.3 mL min -1 . The analytical column was a reversed phase silica based C 18 column (Shim pack CLC ODS). The root exudates were collected through submerging the whole root system into aerated deionized water for 2 hours. The filtered exudate solutions were concentrated to dryness by rotary evaporation at 40 °C, dissolved in 10 mL mobile phase. The chromatographic conditions of organic acid determination were analyzed. The results showed that there was a high selectivity and sensitivity in the organic acid determination by reversed phase high performance liquid chromatography. Coefficients of variation for organic acid determination were lower than 10% except lactic acid. The recoveries were consistently between 80.1% to 108.3%. Detection limits were approximately 0.05 to 4.5 mg L -1 for organic acids except succinic acid with the detection limit of 7.0 mg L -1 . Phosphorus deficiency may contribute to the release of organic acids in soybean root exudates especially malic, lactic and citric acids. 展开更多
关键词 high performance liquid chromatography organic acids root exudates SOYBEAN
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印章色痕形成时间鉴定的GC与HPLC法研究 被引量:1
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作者 蒋仁庆 林俊皓 张振宇 《山东化工》 CAS 2024年第2期147-149,153,共4页
利用气相色谱法和高效液相色谱法对7种印油印章色痕中的挥发性醇类组分和不挥发性红色颜料组分进行检测,以两者含量的比值作为考查指标绘制加热老化和光照老化两种人工老化方式下的老化曲线以及自然老化曲线,总结了印章色痕中醇类组分... 利用气相色谱法和高效液相色谱法对7种印油印章色痕中的挥发性醇类组分和不挥发性红色颜料组分进行检测,以两者含量的比值作为考查指标绘制加热老化和光照老化两种人工老化方式下的老化曲线以及自然老化曲线,总结了印章色痕中醇类组分的挥发规律,为印章色痕形成时间的理化鉴定提供了一种可行的方法。 展开更多
关键词 气相色谱法 高效液相色谱法 印章色痕 形成时间 老化研究
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Determination of Voriconazole in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry: Application in Therapeutic Drug Monitoring
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作者 Waleed Alhussaini Ezzeldeen Ghanem +4 位作者 Magd Alsahly Amani Kurdi Eman Alharbi Imadul Islam Majed Aljeraisy 《American Journal of Analytical Chemistry》 2023年第9期378-389,共12页
A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with flucona... A sensitive, accurate and robust Liquid Chromatography Tandem Mass Spectrometry method has been developed and validated to measure voriconazole trough levels in human plasma. The plasma samples were mixed with fluconazole as an Internal Standard and directed to protein precipitation and drug extraction. An aliquot of 1 μl was injected into the chromatographic system and separated by the Acquity BEH C18 column at a flow rate of 0.30 ml/min in a gradient mobile phase consisting of acetonitrile, Ultrapure water (UPW), methanol and formic acid. Voriconazole was detected by a Triple Quadrupole Detector (TQD) operating on Multiple Reaction Monitoring (MRM) and a positive ion mode Electrospray ionization (ESI) Q1 mass: 350.1 m/z, Q3 mass: 281.1 m/z. Method linearity of the calibration curve (0.10 - 8.00 μg/ml) indicated a correlation coefficient r ≥ 0.99. The intra and inter-assay accuracy was within 85% - 115% and the intra and inter-assay precision was ≤5.76%. Voriconazole recovery percentage was between 97.69 - 119.62%. The method was successively applied in routine voriconazole TDM. 展开更多
关键词 VORICONAZOLE Human Plasma liquid chromatography Tandem Mass Spectrometry Therapeutic Drug Monitoring
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A High-Performance Liquid Chromatography Method for the Simultaneous Determination of Five Index Components in Danhong Injection
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作者 Yun An Tian Tian +2 位作者 Qinglin Wang Xingchu Gong Chenchen Wang 《American Journal of Analytical Chemistry》 CAS 2023年第11期481-492,共12页
The purpose of this study was to establish a high-performance liquid chromatography (HPLC) method for the simultaneous determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, a... The purpose of this study was to establish a high-performance liquid chromatography (HPLC) method for the simultaneous determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid in Danhong injection. The chromatographic method employed was as follows: the column was a Welch Ultimate XB-C18 column (250 mm × 4.6 mm, 10 μm), the mobile phase was a gradient elution of 0.4% formic acid aqueous solution (A) and acetonitrile (B), the detection wavelengths were 280 nm for sodium danshensu, protocatechuic aldehyde, and salvianolic acid B and 326 nm for 4-coumaric acid and rosmarinic acid, the sample volume was 10 μL, the flow rate was 1.0 mL/min, and the column temperature was 35°C. This method can realize the separation and determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid within 50 minutes. The linear relationships of the five peak areas and their concentrations are good (R2> 0.9997). The precision RSD values are all less than 1.0%. The reproducibility RSD values are all less than 1.3%. The stability RSD values are all less than 2.2%. The recovery values ranged from 92.4% to 99.4%. This method is simple, accurate, and reproducible. It can be used for the determination of sodium danshensu, protocatechuic aldehyde, rosmarinic acid, salvianolic acid B, and 4-coumaric acid in Danhong injection. 展开更多
关键词 Danhong Injection High Performance liquid chromatography Phenolic Acid FLAVONOIDS
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Separation of Ephedrines Using 1-Butyl-3-methylimidazolium-tetrafluoroborate Ionic Liquids as Eluent in High-performance Liquid Chromatography (HPLC) 被引量:1
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作者 Li Jun HE, Wen Zhu ZHANG, Bo WEN, Xia LIU, Sheng Xiang JIANG* Lanzhou Institute of Chemical Physics, Chinese Academy of Science, Lanzhou 730000 《Chinese Chemical Letters》 SCIE CAS CSCD 2003年第6期603-604,共2页
A simple, effective HPLC method for separation of ephedrines was achieved by using 1-butyl-3-methylimidazolium-tetrafluoroborate ionic liquid solution (0.1% v/v) as eluent at pH 3.0. The involved mechanism may be due ... A simple, effective HPLC method for separation of ephedrines was achieved by using 1-butyl-3-methylimidazolium-tetrafluoroborate ionic liquid solution (0.1% v/v) as eluent at pH 3.0. The involved mechanism may be due to that the imidazolium cations can effectively shield the silanol groups of alkylsilica surface, thereby decreasing band tailing and increasing the separation efficiency. 展开更多
关键词 Ionic liquid EPHEDRINE hplc.
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