共查询到20条相似文献,搜索用时 281 毫秒
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提出了由双泵单阀的驱动系统和双柱(预处理柱和分析柱)切换的分析系统所组成的色谱分析流程并应用于测定抗病毒口服液中非法添加物利巴韦林.样品离心后取上清液直接进样于C18预处理柱,水作为预处理流动相;用0.3 g·L-1磷酸二氢钠溶液(分析流动相)将保留在预处理柱上的药物冲入Kromasil C18分析柱(250 mm×4.6 mm,5μm)进行测定.方法集样品净化和色谱分析一次连续进行,测定条件下无干扰.检测波长205.6 am,药物的质量浓度在0.4~40.0 mg·L-1范围内呈线性(r=0.999 2),检出限(S/N=3)为0.08 mg·L-1,加标回收率分别为98.32%,98.45%,99.45%. 相似文献
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高效液相色谱法测定小儿化痰止咳颗粒中盐酸麻黄碱的含量 总被引:1,自引:0,他引:1
目的:测定小儿化痰止咳颗粒中盐酸麻黄碱的含量.方法:采用高效液相色谱法.色谱柱为Kromasil C18柱(250 mm×4.6 mm,5μm);乙腈-0.02%磷酸二氢钠溶液(含0.1%三乙胺,磷酸调pH 2.7)(5∶95)为流动相,流速为1.0 mL/min;检测波长210 nm.结果:盐酸麻黄碱在0.2~4.0μg范围内具有良好线性关系,平均回收率为98.61%,RSD为0.97%.结论:该法可用于小儿化痰止咳颗粒中盐酸麻黄碱的含量测定. 相似文献
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高效液相色谱法测定鸡肉中己烯雌酚 总被引:1,自引:0,他引:1
采用高效液相色谱法(HPLC)测定鸡肉中己烯雌酚残留量,将碎鸡肉用甲醇超声提取,合并提取液浓缩近干,用甲醇溶解残渣,所得溶液用于 HPLC 测定.Symmetry C,18用作色谱柱,甲醇与0.012 8 mol·L-1 磷酸二氢钠溶液以63比37(体积比)混合后作为流动相,流速为 1.0 mL·min-1.在230 nm波长处,用二极管阵列检测器检测.对鸡肉样品作了分析,测定结果的相对标准偏差(n=5)均小于 10%,回收试验给出回收率在 87.5%~92.3%之间.测得方法的检出限(S/N=3)为 20 μg·kg-1. 相似文献
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提出了高效液相色谱法测定烟草中有机酸含量的方法。烟草样品经0.1 mol.L-1氢氧化钠溶液高速匀浆提取,提取液通过装有MCI-GEL反相树脂固相萃取小柱净化,以ZORBAXStable Bound色谱柱(4.6 mm×150 mm,1.8μm)为固定相,0.01 mol.L-1磷酸二氢钠溶液(pH2.98)和乙腈(98+2)溶液为流动相梯度洗脱,用二极管阵列检测器于210 nm波长处检测。烟草中主要的有机酸均在12 min内达到基线分离,方法加标回收率在95.0%~103.0%之间,相对标准偏差(n=7)在1.8%~2.8%之间。 相似文献
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反相高效液相色谱法测定烧伤大鼠体内的肠三叶因子 总被引:1,自引:0,他引:1
采用反相高效液相色谱法测定烧伤大鼠体内的肠三叶因子 (ITF) ,其中色谱柱为HypersilC4柱 ( 4 6mmi.d .× 2 5 0mm ,柱填料的孔径为 3 0nm ,粒度为 5 μm) ,流动相为乙腈 水 (含体积分数为 0 1%的三氟乙酸 )溶液 ,梯度洗脱 ,流速为 1mL/min。在 2 14nm检测波长下 ,ITF在 1mg/L~ 10 0mg/L时具有良好的线性关系 ,相关系数为0 9989,最低检测限为 0 5mg/L。ITF的加标回收率为 93 95 %~ 10 5 90 % ,日内测定结果的RSD <5 3 3 % ,日间测定结果的RSD <6 10 %。方法准确、灵敏 ,可作为一种有效的分析手段。 相似文献
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高效液相色谱法同时测定诺诺感冒片中扑尔敏、扑热息痛、盐酸伪麻黄碱的含量 总被引:8,自引:1,他引:7
采用反相高效液相色谱法 ,在C18柱上以V(甲醇 )∶V(水 ) =2 5∶75的溶液为流动相 (内含 0 .0 5mol/L磷酸二氢钠 ) ,检测波长为 2 0 5nm ,同时分离测定诺诺感冒片中扑尔敏、扑热息痛、盐酸伪麻黄碱的含量。扑尔敏、扑热息痛和盐酸伪麻黄碱的检出限分别为 1.16mg/L ,0 .15mg/L和 1.82mg/L ,其相应的回收率分别为 98.35 % (n =5 ,RSD =1.6 0 % ) ,10 1.16 % (n =5 ,RSD =1.5 0 % )和 98.5 0 % (n =5 ,RSD =1.5 9% )。方法简便、快速 ,重现性好 ,适用于诺诺感冒片的质量检验分析。 相似文献
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高效液相色谱同时测定饲料中三种抗生素 总被引:3,自引:0,他引:3
建立了反相高效液相色谱法同时检测饲料中土霉素、四环素、金霉素的方法.色谱柱为AichromBond-AQ C18柱,150×4.6mm,粒度5μm;流动相:0.01mol/L磷酸二氢钠溶液(pH2.5)+乙氰,采用梯度洗脱,乙氰浓度在0~13min内由13%上升到40%;柱温35℃;流速为1.0mL/min;进样量101μL;检测波长375nm.方法检出限:土霉素和四环素0.25μg/mL、金霉素0.50μg/mL,回收率91.70%~101.19%,RSD<1.39%(n=7). 相似文献
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Emara S Morita I Tamura K Razee S Masujima T Mohamed HA El-Gizawy SM El-Rabbat NA 《Talanta》1994,41(11):1973-1980
Adriamycin, adriamycinol, adriamycinone and duanorubicin were simultaneously determined by the development of an on-line plasma clean-up system. A short protein-coated Lichrosorb, RP-8, RP-2, CN and muBondapak phenyl as well as ODS silica have been examined for their performance as pre-columns. The drugs and metabolites were separated from weakly retained plasma components through two steps; phosphate buffer saline, pH 7.4 and 15% acetonitrile in 0.1 M sodium dihydrogen phosphate, pH 3. The chromatographic conditions were: ODS/TM column, flow rate 1 ml/min, 35% acctonitrile in 0.1 M sodium dihydrogen phosphate (pH 3) containing 0.3% heptafluorobutyric acid as mobile phase. The detection was carried out using fluorescence monitor operated at an emission 555 nm and excitation 460 nm. Good resolution was obtained within 13 min. This method is reproducible for analysis of drugs and metabolites (99.3-100.1%, CV < 2%) in plasma. 相似文献
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A high-performance liquid chromatographic (HPLC) method for determining glycarbylamide (GB) in chicken tissue was developed. GB was extracted with acetonitrile, followed by solid-phase extraction cleanup using a Bond Elut cartridge column with neutral alumina. After the extract had been evaporated to dryness, the residue was dissolved in 1.0 mL 0.1 N sodium hydroxide. Then 1.0 mL 0.1 M potassium dihydrogen phosphate solution was added to it. HPLC separation was done on a 250 x 4.6 mm id TSK-GEL ODS 80 column with 0.05M potassium dihydrogen phosphate as the mobile phase. Ultraviolet detection was done at a wavelength of 260 nm. The calibration curve of standard GB solutions was linear between 0.16 and 3 micrograms/mL (correlation coefficient, r = 0.999). The recovery of GB from chicken muscle spiked at 0.8 microgram/g was 88.6 +/- 2.3% (mean +/- standard deviation, n = 5), and the lower limit of determination was 0.05 microgram/g in chicken muscle. 相似文献
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The chromatographic behaviour of azobenzene and fourteen of its derivatives was studied by reversed-phase high-performance liquid chromatography with a C18 stationary phase. The optimal composition of the mobile phase is 9:1 methanol-0.01 M aqueous sodium dihydrogen phosphate which is 0.0002 M in ethylenediaminetetraacetic acid, with a pH of 4.5. The solutes can be detected spectrophotometrically, voltammetrically or polarographically. Spectrophotometric measurement in the visible range is more sensitive than in the UV range (detection limits of 0.04-0.1 ng at 410 nm compared with 0.3-0.5 ng at 265 nm). Voltammetric detection is highly sensitive for hydroxy and amino derivatives [detection limits 0.02-0.09 ng at +0.8 V (Ag-AgCl)], whereas for other substances the detection limits are a few nanograms. Polarographic detection is the least sensitive [detection limits 4-8 ng at -0.6 V (Ag-AgCl)]. All the calibration graphs exhibit good linearity, but spectrophotometric detection yields a wider linear dynamic range. Voltammetric detection is more precise at low solute concentrations (relative standard deviations of the peak heights 0.5-1.0% and 1.0-1.5% for voltammetric and spectrophotometric detection, respectively, with amounts of solute from 1 to 10 ng). 相似文献
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固相萃取和高效液相色谱相结合快速测定苦瓜甙A的含量(英文) 总被引:11,自引:0,他引:11
建立了一个快速、简单、准确的固相萃取和高效液相色谱相结合的测定苦瓜甙A含量的方法。样品经石墨碳固相萃取管 (3mL/ 2 5 0mg)纯化后以高效液相色谱检测。色谱柱为C18,流动相为V(乙腈 )∶V(甲醇 )∶V(5 0mmol/L磷酸二氢钾缓冲液 ) =2 5∶2 0∶6 0 ,流速为 0 .8mL/min ,检测波长为 2 0 8nm。标准曲线自 10mg/L到 10 0 0mg/L呈线形关系 (r2 =0 .9992 )。该方法具有很好的重现性 ,日内或日间的相对标准偏差和相对平均误差均小于 10 %。样品回收率大于 90 %。 相似文献
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A previously established mobile phase composition for a high-performance liquid chromatography (HPLC)-electrochemical detection (ED) method for the determination of Brazilein is further examined by HPLC-UV. Each component in the mobile phase is evaluated by the HPLC-UV system, and a convenient HPLC-UV method for the determination of Brazilein is developed. The mobile phase of this HPLC-UV method consists of sodium dihydrogen phosphate (NaH(2)PO(4)). The detection limit of Brazilein (signal-to-noise = 3) is 1 ng, and the calibration graph of Brazilein ranges from 1-120 ng per 20-microL injection. The validity of the proposed HPLC-UV method is demonstrated by the analysis of Brazilein in real plant samples. The differences between the HPLC-ED method and the proposed HPLC-UV method are given. 相似文献
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An efficient pressurized capillary electrochromatography (pCEC) method has been successfully developed for the determination of six catechins in tea. The separation was performed on a reversed-phase EP-100-20/45-3-C18 capillary column (total length of 45?cm, effective length of 20?cm, diameter of 100?μm, ODS packing inside for 3?μm). The mobile phase ratio of organic phase, the concentration of phosphate buffer and sodium heptanesulfonate, separation voltage, and other experimental conditions were investigated and optimized. The mobile phase was 15?mM NaH2PO4 and 12?mM sodium heptanesulfonate (pH 3.0)/methanol (64:36) at a flow rate of 0.04?mL/min. Under optimal conditions including applied voltage of ?4?kV and a UV detection wavelength of 230?nm, the six catechins in the tea were well separated. The calibration curves for the analytes had good linearity in the range of 8.02?μg/mL–202.13?μg/mL with a correlation coefficient of 0.9928–0.9997. The limits of detection (LOD) for the six catechins were 4.62?μg/mL–11.63?μg/mL (S/N?=?3). The recoveries of the six catechins were 96.2%–108.4% with a relative standard deviation (RSD) between 0.78% and 4.51%. The method has been used for the determination of six catechins in tea samples with good results. 相似文献
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建立了化妆品中维生素C及其3种衍生物(抗坏血酸葡糖苷(AA-2G)、抗坏血酸磷酸酯镁(AA-2P)、抗坏血酸乙基醚(Only VCE))的高效液相色谱分析方法。化妆水、水乳液等含油脂较少的样品先采用30 mL 0.02 mol/L磷酸二氢钾溶液(pH 3.0)直接提取,然后定容至50 mL;面膏等含油脂较高及凝胶类、啫喱类的样品先加入1.0 mL二氯甲烷分散均匀后再加25 mL 0.02 mol/L磷酸二氢钾溶液(pH 3.0)提取。提取液在12000 r/min下离心后用0.22 μm滤膜过滤。样品分析采用YMC-Triart C18色谱柱,以0.02 mol/L磷酸二氢钾溶液(pH 3.0)和甲醇溶液为流动相,梯度洗脱,流速为1.0 mL/min,柱温为25 ℃,使用二极管阵列检测器(DAD)检测,检测波长为250 nm,外标法定量。结果显示:4种化合物在其线性范围内线性关系良好,相关系数(r2)均大于0.9999;方法的定量限(以信噪比为10计)为0.04~0.08 g/kg;添加水平为0.25~5.0 g/kg时的回收率为95.6%~101.0%,相对标准偏差为0.62%~3.0%。该方法前处理简单、回收率高、精密度好,适用于化妆品中维生素C及其衍生物的测定。 相似文献
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《Analytical letters》2012,45(14):2267-2274
A simple and sensitive liquid chromatography assay following solid phase extraction was developed for simultaneous determination of adenosine and inosine in sheep plasma. The system consisted of a Symmetry C18 column, a mobile phase composed of acetonitrile, 100 mM sodium dihydrogen phosphate and water, and ultraviolet detection at 254 nm. The method showed good sensitivity (limits of detection for adenosine and inosine were 30 and 50 ng/ml, respectively, in the plasma samples), repeatability, and linearity. The developed method was applied to sheep plasma samples from a study examining the cardio active potential of the combination of adenosine and inosine. 相似文献