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Zhang‐Jie Huang Xiang‐Jun Yang Qun‐Yan Wei Qiu‐Fen Hu Jing Chen Guang‐Yu Yang 《中国化学会会志》2005,52(6):1095-1099
In this paper, a new method for the simultaneous determination of palladium and platinum ions was developed using a rapid column high performance liquid chromatograph equipped with an on‐line enrichment technique. The palladium and platinum ions were pre‐column derivatized with 5‐(p‐aminobenzylidene)‐thiorhodanine (ABTR) to form colored chelates. The Pd‐ABTR, Pt‐ABTR chelates can be absorbed onto the front of an enrichment column when they were injected into the injector and sent to the enrichment column [ZORBAX Stable Bound, 4.6 × 10 mm, 1.8 μm] with a buffer solution of 0.05 mol/L sodium acetate‐acetic acid buffer solution (pH 3.5) as mobile phase. After the enrichment had finished, by switching the six‐ports switching valve, the retained chelates were back‐flushed by mobile phase and traveled towards the analytical column. These chelates separation on the analytical column [ZORBAX Stable Bound, 4.6 × 50 mm, 1.8 μm] was satisfactory with 65% methanol (containing 0.05 mol/L of pH 3.5 sodium acetate‐acetic acid buffer salt and 0.01 mol/L of tritonX‐100) as mobile phase. The palladium and platinum were separated completely within 2 min. The detection limits (S/N = 3) of palladium and platinum are 1.4 ng/L and 1.6 ng/L, respectively. This method was applied to the determination of palladium and platinum in water and urine samples with good results. 相似文献
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《Analytical letters》2012,45(14):2463-2474
Abstract In this paper, 2‐carboxyl‐1‐naphthalthiorhodamine (CNTR) was synthesized, and a new method for the simultaneous determination of palladium, platinum, and rhodium ions as metal‐CNTR chelates was developed using rapid column high performance liquid chromatography combined with on‐line enrichment. The palladium, platinum, and rhodium ions were precolumn derivatized with CNTR to form colored chelates. The Pb‐CNTR, Pt‐CNTR, and Rh‐CNTR chelates could be absorbed onto the front of the enrichment column when they were injected into the injector and sent to the enrichment column (ZORBAX Stable Bound, 4.6×10 mm, 1.8 µm) with a buffer solution of 0.05 mol/L sodium acetate–acetic acid buffer solution (pH 3.5) as mobile phase. After enrichment, and by switching the six ports switching valve, the retained chelates were back‐flushed by mobile phase and traveling towards the analytical column. The separation of these chelates on the analytical column (ZORBAX Stable Bound, 4.6×50 mm, 1.8 µm) was satisfactory with 54% methanol (v/v) in 0.05 mol/L sodium acetate buffer (pH 3.5) containing 1 g/L Triton X‐100 as mobile phase. Palladium, platinum, and rhodium were separated completely within 2 min. The detection limits (S/N=3) of palladium, platinum, and rhodium are 1.4 ng/L, 1.2 ng/L, and 1.8 ng/L, respectively. This method was applied to the determination of palladium, platinum, and rhodium in water, urine, and soil samples with good results. 相似文献
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An improved HPLC method was developed for the determination of piperacillin and tazobactam in human plasma and pharmacokinetic study in Chinese healthy volunteers. Piperacillin and tazobactam in human plasma were extracted by solid-phase extraction and separated on a C(18) column and detected at 220 nm. The mobile phase for piepracillin consisted of 0.01 mol/L sodium dihydrogen phosphate (pH = 4.65) and acetonitrile (71:29, v/v), and that for tazobactam was 0.05 mol/L sodium dihydrogen phosphate (pH = 4.45) and methanol (90:10, v/v). The method was linear in the range 0.25-320.00 microg/mL for piperacillin (r(2) = 0.995) and 0.25-64.00 microg/mL for tazobactam (r(2) = 0.994). The lower limit of quantification of both compounds was 0.25 microg/mL. The intra- and inter-day precisions of piperacillin and tazobactam at three concentrations were all less than 9.2% and accuracies were within the range 97.0-108.0%. The method was used to investigate the pharmacokinetics of piperacillin and tazobactam in 12 volunteers who were intravenously given a dosage of 1.25, 2.50 and 3.75 g in three periods. The results showed that piperacillin sodium-tazobactom sodium (4:1) for injection in Chinese people fits linear dynamics, and the administred dosage can be adjusted with therapeutic effect. 相似文献
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T Oshima K Sagara Y Y Tong G Zhang Y H Chen 《Chemical & pharmaceutical bulletin》1989,37(9):2456-2458
A new ion-pair high-performance liquid chromatographic method for the analysis of hyoscyamine and scopolamine in various kinds of crude drugs derived from solanaceous plants was evaluated using sodium dodecyl sulfate as a counter ion. A reversed-phase chromatographic system consisting of a chemically bonded ODS silica gel column with phosphate buffer (pH 2.5)-acetonitrile (65:35) containing 17.5 mM sodium dodecyl sulfate as the mobile phase was used. Hyoscyamine and scopolamine in crude drugs derived from Scopolia, Atropa, Hyoscyamus and Datura species were separated from other compounds in the crude drugs and determined within 20 min after direct injection of the solution extracted with the mobile phase. The results for various kinds of samples are presented. 相似文献
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基于高速逆流色谱(HSCCC)技术从玛咖中分离制备出两种芥子油苷,苄基芥子油苷(glucotropaeolin, GTL)和甲氧基苄基芥子油苷(glucolimnanthin, GLI)。使用正交设计试验对分离条件进行优化,采用高分辨质谱对制备的组分进行鉴定,采用高效液相色谱法(HPLC)对组分进行定量分析。确定了两个组分GTL与GLI的HSCCC最佳分离条件:溶剂系统为正丁醇-乙腈-200 g/L硫酸铵溶液(1:0.5:2.4, v/v/v),上相为固定相,下相为流动相,流动相流速2 mL/min,主机转速900 r/min,从玛咖根粗提物中一次性分离得到157.72 mg/kg纯度为97.9%的苄基芥子油苷和31.93 mg/kg的甲氧基苄基芥子油苷,固定相保留率达57.6%。该方法成本低,简便易行,样品损失量小,可大量循环进样制备。 相似文献
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Recycling high speed counter-current chromatography (HSCCC) was successfully applied to resolution of (R, S)-naproxen (NAP) using hydroxypropyl-β-cyclodextrin (HP-β-CD) as chiral selector. The two-phase solvent system composed of n-hexane-ethyl acetate-0.1 mol L(-1) phosphate buffer solution with pH=2.67 (8:2:10, v/v/v) was selected. Influence factors for the chiral separation process were investigated, including concentration of HP-β-CD, equilibrium temperature and pH of aqueous phase. Suitable elution mode was selected for HSCCC enantioseparation of (R, S)-NAP. Under optimum separation conditions, 29 mg of (R, S)-NAP was separated using preparative recycling HSCCC with the molar ratio HP-β-CD/NAP racemate 83:1. Technical details for recycling elution mode were discussed as for chiral HSCCC separation. The purities of both (S)-NAP and (R)-NAP were over 99.5% as determined by HPLC. Enantiomeric excess of (S)-NAP and (R)-NAP reached 99.4%. Recovery for NAP enantiomers from HSCCC fractions was 82-89%, yielding 13 mg of (S)-NAP and 12 mg of (R)-NAP. 相似文献
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This paper reports the utilization of solid phase extraction and the reversed‐phase high‐performance liquid chromatography (RP‐HPLC) for the determination of six transition metal ions (iron, cobalt, nickel, copper, zinc and manganese) in biological samples. The samples were digested by microwave digestion. The iron, cobalt, nickel, copper, zinc and manganese ions in the digested samples can react with 2‐(2‐quinolinylazo)‐5‐diethylaminophenol (QADEAP) to form colored chelates in pH 4.0 acetic acid‐sodium acetic buffer solutions and cetyl trimethylammonium bromide (CTMAB) medium. These chelates were enriched by solid phase extraction with C18 cartridge. Then the chelates were separated on a Waters Nova‐Pak‐C18 column (3.9 × 150 mm, 5 μm) by gradient elution with methanol (containing 0.5% of acetic acid and 0.1% of CTMAB) and 0.05 mol/L pH 4.0 acetic acid‐sodium acetic buffer solution (containing 0.1% of CTMAB) as mobile phase at a flow rate of 0.5 mL/min. The detection limits of iron, cobalt, nickel, copper, zinc and manganese are 3 ng/L, 4 ng/L, 2 ng/L, 4 ng/L, 8 ng/L, 10 ng/L, respectively. This method was applied to the determination of iron, cobalt, nickel, copper, zinc and manganese in biological samples with good results. 相似文献
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A high-performance liquid chromatographic multiresidue method was developed for the determination of 8 penicillin compounds (benzylpenicillin, phenoxymethylpenicillin, ampicillin, amoxicillin, nafcillin, oxacillin, cloxacillin, and dicloxacillin) at trace levels in muscle tissue. This method involves extraction of the penicillins with phosphate buffer pH 9 followed by cleanup and concentration on a C18 solid-phase extraction column and reaction with benzoic anhydride at 50 degrees C for 5 min and with 1,2,4-triazole and mercury(II) chloride solution pH 9 at 65 degrees C for 10 min. The derivatized compounds are eluted on a C8 column with a mobile phase containing acetonitrile and phosphate buffer (pH 6; 0.1 mol/L) loaded with sodium thiosulfate and ion-pairing tetrabutylammonium hydrogenosulphate. The method detection limit is approximately 3-11 micrograms/kg and the limit of determination was evaluated down to 25 micrograms/kg in line with the criteria of the EU decision No. 93/256/EEC. 相似文献
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Determination of amino acid neurotransmitters in rat hippocampi by HPLC‐UV using NBD‐F as a derivative
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Xiaomeng Wu Rui Wang Qingqing Jiang Shue Wang Yao Yao Lihua Shao 《Biomedical chromatography : BMC》2014,28(4):459-462
A simple, rapid and accurate high‐performance liquid chromatography method with ultraviolet–visible detection was developed for the determination of five amino acid neurotransmitters – aspartate, glutamic acid, glycine, taurine and γ‐aminobutyric acid – in rat hippocampi with pre‐column derivatization with 4‐fluoro‐7‐nitrobenzofurazan. Several conditions which influenced derivatization and separation, such as pH, temperature, acetonitrile percentage mobile phase and flow rate, were optimized to obtain a suitable protocol for amino acids quantification in samples. The separation of the five neurotransmitter derivatives was performed on a C18 column using a mobile phase consisting of phosphate buffer (0.02 mol/L, pH 6.0)–acetonitrile (84:16, v/v) at a flow rate of 1.0 mL/min with the column temperature at 30°C. The detection wavelength was 472 nm. Without gradient elution, the five neurotransmitter derivatives were completely separated within 15 min. The linear relation was good in the range from 0.50 to 500 µmol/L, and the correlation coefficients were ≥0.999. Intra‐day precision was between 1.8 and 3.2%, and inter‐day precision was between 2.4 and 4.7%. The limits of detection (signal‐to‐noise ratio 3) were from 0.02 to 0.15 µmol/L. The established method was used to determine amino acid neurotransmitters in rat hippocampi with satisfactory recoveries varying from 94.9 to 105.2%. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献
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Gan Zhou Shuyun Shi Wei Zhang Zhirong Tan Yao Chen Dong Guo Honghao Zhou Haitang Hu Jin Tan 《Biomedical chromatography : BMC》2010,24(10):1130-1135
Ilaprazole is a new proton pump inhibitor designed for the treatment of gastric ulcers, and limited data is available on the metabolism of the drug. In this article, the structural elucidation of urinary metabolites of ilaprazole in human was described by HPLC‐ESI‐MS/MS and stopped‐flow HPLC‐NMR experiments. Urinary samples were precipitated by sodium carbonate solution, and then extracted by liquid–liquid extraction after adding ammonium acetate buffer solution. The enriched sample was separated using a C18 reversed‐phase column with the mobile phase composed of acetonitrile and 0.05 mol/L ammonium acetate buffer solution in a gradient solution, and then directly coupled to ESI‐MS/MS detection in an on‐line mode or 1H‐NMR (500 MHz) spectroscopic detection in a stopped‐flow mode. As a result, four sulfide metabolites, ilaprazole sulfide (M1), 12‐hydroxy‐ilaprazole sulfide (M2), 11,12‐dihydroxy‐ilaprazole sulfide (M3) and ilaprazole sulfide A (M4), were identified by comparing their MS/MS and NMR data with those of the parent drug and available standard compounds. The main biotransformation reactions of ilaprazole were reduction and the aromatic hydroxylation of the parent drug and its relative metabolites. The result testified that HPLC‐ESI‐MS/MS and HPLC‐NMR could be widely applied in detection and identification of novel metabolites. Copyright © 2010 John Wiley & Sons, Ltd. 相似文献
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用液相等电聚焦电泳纯化藻蓝蛋白亚基 总被引:5,自引:0,他引:5
以纯藻蓝蛋白(C-phycocyanin, C-PC)为材料, 采用Rotofor系统进行液相等电聚焦(Liquid-phase isoeletric focusing, LP-IEF)电泳纯化C-PC的α, β亚基, 探讨蛋白质亚基纯化的制备电泳(Preparative eletrophoresis)技术. 结果显示, 样品经2次等电聚焦电泳后, C-PC 的α, β亚基分别浓集在pH=4.9和pH=4.1附近, 平板超薄等电聚焦(Slab ultra thin IEF)和SDS-PAGE电泳鉴定表明分别为高纯度的C-PC α, β亚基. 提示LP-IEF是分离纯化等电点差异蛋白质活性亚基的简便有效的方法. 相似文献
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Determination of human plasma protein binding of baicalin by ultrafiltration and high-performance liquid chromatography 总被引:2,自引:0,他引:2
A simple and selective HPLC assay was developed and utilized for determination of human plasma protein binding of baicalin. The method involved solid-phase extraction and reversed-phase chromatographic separation with a mobile phase of acetonitrile-0.02 mol/L phosphate buffer (pH 2.5; 25:75, v/v) and UV detection at 276 nm. The standard curve for baicalin was linear over the concentration range 0.1-20 microg/mL and the limit of detection was 0.02 microg/mL. The absolute recovery was greater than 76%. The intra-day and inter-day variations were less than 10%. Ultrafiltration technique was applied to determining the plasma protein binding of baicalin in human plasma. Results show the plasma protein binding of baicalin was in the range 86-92% over all the concentrations studied and the protein binding association constant was determined to be 1.21 x 10(5) L/mol at 4 degrees C. 相似文献
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A high-performance liquid chromatographic method with electrochemical detection (HPLC-ED) at a boron-doped diamond film electrode with preliminary separation and preconcentration by solid-phase extraction (SPE) has been developed for the determination of 1-hydroxypyrene (1-HP) in human urine. 1-HP is among the most widely used biomarkers of exposure to polycyclic aromatic hydrocarbons. Optimal HPLC-ED conditions have been found: mobile phase methanol-0.05 mol L(-1) phosphate buffer pH 5.0 (80:20, v/v), detection potential +1,000 mV versus Ag/AgCl (3 mol L(-1) KCl), and flow rate 0.8 mL min(-1). For SPE, LiChrolut(?) RP-18 E cartridges were used. The extraction yield was (87.0 ± 5.8)% (n = 5). The concentration dependence of 1-HP was measured in the concentration range from 0.01 to 10 μmol L(-1) (2.18-2,180 μg L(-1)) using methanolic solutions resulting from the SPE pretreatment of spiked human urine samples. The limit of detection (signal-to-noise ratio 3) and the limit of quantification (signal-to-noise ratio 10) of the biomarker were 0.013 μmol L(-1) (2.84 μg L(-1)) and 0.043 μmol L(-1) (9.39 μg L(-1)), respectively, which is sufficient for its determination in the urine of persons exposed to polycyclic aromatic hydrocarbons. 相似文献
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A rapid and sensitive CEC method with methacrylate ester‐based monolithic column has been developed for separation and determination of five coumarins (byakangelicin, oxypeucedanin hydrate, xanthotoxol, 5‐hydroxy‐8‐methoxypsoralen and bergapten) in Angelica dahurica extract. Surfactant sodium desoxycholate (SDC) was introduced into the mobile phase as the pseudostationary to dynamically increase the selectivity of analytes instead of increasing the hydrophobicity of stationary phase. In addition, other factors, pH of phosphate buffer, ACN content and applied voltage, for instance, have also an obvious effect on the resolution but little on the retention time. Satisfactory separation of these five coumarins was achieved within 6 min under a 30:70 v/v ACN–buffer containing 20 mM sodium dihydrogen phosphate (NaH2PO4) and 0.25 mM SDC at pH 2.51. The RSDs of intraday and interday for relative peak areas were less than 3.0% and 4.7%, respectively; and the recoveries were between 87.5% and 95.0%. The LODs were lower than 0.15 μg/mL and the LOQs were lower than 0.30 μg/mL, respectively, while calibration curves showed a good linearity (r2 > 0.9979). Finally, five target coumarins from the crude extracts of A. dahurica were separated, purified, and concentrated by D‐101 macroporous resin, and were successfully separated and quantitatively determined within 6 min. 相似文献