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反相高效液相色谱检测丹参药材中4种丹参酮的含量 总被引:6,自引:0,他引:6
建立了测定丹参药材中4种丹参酮含量的反相高效液相色谱法,色谱条件:流动相为水(含0.5%三乙胺)-甲醇-四氢呋喃(45/55/5,V/V/V),流速为1mL/min;PDA检测波长254m;4种成分丹参酮Ⅰ、丹参酮ⅡA、隐丹参酮和二氢丹参酮的加样回收率在95.1%-101.2%之间,线性范围为0.08-2μg。该方法准确,稳定,重现性好。根据该色谱条件,测定了不同产地的丹参药材,结果表明:该色谱方法准确检测了生药中4种丹参酮的含量,适合于丹参药材的质量控制。 相似文献
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用阳离子交换树脂CM-52分离纯化类人胶原蛋白Ⅱ(Human Collagen-like Bioprotein Ⅱ,HCBⅡ)。通过实验,分别确定了静态吸附和柱层析吸附的操作条件,即静态吸附:在pH4.0、NaCl0.15mol/L、进料浓度7g/L,处理量17.26ml/g树脂的条件下进行吸附,吸附时间为60min;柱层析:在pH4.0、NaCl0.15mol/L、进料浓度5g/L、流速5ml/min的条件下进行吸附。然后上柱,在pH4.0、NaCl0.30mol/L下进行脱附。实验表明,采用静态吸附的方式吸附HCBⅡ,然后上柱洗脱,HCBⅡ的吸附量可达到48、6mg/g树脂,回收率83.8%,操作时间短,分辨率高,最终纯化的HCBⅡ达电泳纯,分子量为97kD。 相似文献
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反相高效液相色谱法测定人血浆中利培酮及其代谢物的质量浓度 总被引:3,自引:0,他引:3
建立了测定人血浆中利培酮及其活性代谢物9-羟利培酮质量浓度的反相高效液相色谱方法。用Zor-baxODSC18色谱柱,以V(甲醇):V(水):V(1mol/L醋酸铵):V(3mol/L氨水)=300:50:3:1为流动相,检测波长为280nm,流速为0.8mL/min。利培酮的线性范围为2~600μg/L(r=0.996),回收率为(98.2±3.5)%,日内与日间的标准偏差分别为4.12%和4.83%;9-羟利培酮的线性范围为2~800μg/L(r=0.998),回收率为(97.8±3.8)%,日内与日间的标准偏差分别为4.28%和4.81%。 相似文献
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高效液相色谱法测定生姜中的6-姜酚 总被引:7,自引:0,他引:7
用C18色谱柱,以V(甲醇):V(水):V(冰乙酸)=35:64:1溶液作流动相,进样量5μL,在流速1.0mL/min下,可不经分离直接测定生姜中的6-姜酚。方法RSD小于1.00%,回收率97%~102%,相关系数0.9999。 相似文献
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Adalet Tunçeli Gülay Ocak Ali Rehber Türker 《International journal of environmental analytical chemistry》2015,95(14):1395-1411
A solid phase extraction (SPE) procedure based on Amberlite IRA 900 resin was developed for speciation and separation of inorganic arsenic species (III, V) and total As in water samples. The As species and total As in eluent solutions were determined by electrothermal atomic absorption spectrometry (ETAAS) using Ni chemical modifier with 1200°C pyrolysis temperature. Experimental parameters such as pH value, sample volume, flow rate, volume and concentration of eluent solution for As(V) were optimised and 98.0 ± 1.9% recovery was found at pH 4.0. Experimental adsorption capacity of the resin for As(V) was investigated and 229.9 mg g–1 was found. Under optimised experimental conditions, instrumental parameters such as limit of detection (LOD) and limit of quantification (LOQ) found were 0.126 and 0.420 µg L–1, respectively. Interference effects of coexisting ions in the sample matrix on the recovery of As(V) were investigated. Concentration of As(III) was obtained by subtracting As(V) concentration found at pH 4.0 from total As(III + V) found at pH 8.0. The accuracy of the method proposed by using the resin was tested for analysing As species in a waste water standard reference material (SRM, CWW-TM-D) and spiked real water samples with recovery above 95%. The method proposed was also applied to the determinations of As species and total As in underground hot waters and tap water with relative error below 3%. 相似文献
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建立了高效液相色谱法(HPLC)检测小麦籽粒中化学杂交剂SQ-1主成分杀雄嗪酸残留的方法。以75%乙醇为提取剂,正反萃取净化;采用Diamonsil C18不锈钢柱,以甲醇-0.5%(NH4)2HPO4溶液(60∶40,V/V,pH 2.5)为流动相,检测波长283 nm,流速1.0 mL/min。结果表明:化学杂交剂SQ-1主成分杀雄嗪酸在0.75~25.0 mg/L范围内线性关系良好,相关系数r=0.9999,在3个添加水平(1.0,5.0和10.0 mg/kg)范围内,平均加标回收率在84.2%~95.0%之间,相对标准偏差为1.0%~3.3%,检出限为0.075 mg/L。 相似文献
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A. Nilchi T. Shariati Dehaghan S. Rasouli Garmarodi 《Journal of Radioanalytical and Nuclear Chemistry》2013,295(3):2111-2115
A simple and reliable method for rapid extraction and determination of uranium and thorium using octadecyl-bonded silica modified with Cyanex 302 is presented. Extraction efficiency and the influence of various parameters such as aqueous phase pH, flow rate of sample solution and amount of extractant has been investigated. The study showed that the extraction of uranium and thorium increase with increasing pH value and was found to be quantitative at pH 6; and the retention of ions was not affected significantly by the flow rate of sample solution. The extraction percent were found to be 89.55 and 86.27 % for uranium and thorium, respectively. The maximal capacity of the cartridges modified by 30 mg of Cyanex 302 was found to be 20 mg of uranium and thorium. The method was successfully applied to the extraction and determination of uranium and thorium in aqueous solutions. The percentage recovery of uranium and thorium in a number of natural as well as seawater samples of Iran were also investigated and found to be in the range of 85–95 %. 相似文献
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A new method for benzocaine determination employing FIA and HPLC with electrochemical detection on a carbon paste electrode was developed. The optimum conditions for the determination were found. Carrier solution for FIA consisted of B–R buffer pH 4 (80 % methanol, v/v) and used flow rate was 1.0 mL min?1. Mobile phase for HPLC consisted of B–R buffer pH 4 (75 % methanol, v/v) with flow rate 0.4 mL min?1. Working potential of +1.2 V was employed. Practical applicability of the methods was tested on the determination of benzocaine in selected pharmaceuticals. The results were in agreement with results obtained using spectrophotometric detection and with one exception also with the content declared by the manufacturer. 相似文献
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A method is described for measurement of freely dissolved copper concentrations in natural water samples using supported liquid membrane (SLM) extraction under equilibrium conditions, a technique denoted equilibrium sampling through membranes (ESTM). For this purpose, 1,10-dibenzyl-1,10-diaza-18-crown-6 as neutral carrier and oleic acid were used in the membrane phase. The main variables optimised were the carrier used to form the metal complexes, the organic solvent used in the membrane, the countercation, pH, the ligand used in the acceptor phase, the extraction time, and the flow rate of the donor phase. After the optimisation process an enrichment factor of 18.5 was obtained. Equilibrium conditions were reached after extraction for 60 min if a flow rate of 1.0 mL min–1 or greater was used. When different ligands such as humic acids, phthalic acid, and EDTA were added to the sample solution, and sample pH ranged from 6 to 8, the results obtained for freely dissolved copper concentrations were in a good agreement with results from speciation calculations performed with Visual Minteq V 2.30, Cheaqs V L20.1, and WinHumic V. The developed technique was applied to analysis of stream and leachate water.Electronic Supplementary Material Supplementary material is available for this article at 相似文献
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液相色谱-串联质谱法测定水产品中麻醉剂MS-222残留 总被引:3,自引:0,他引:3
建立了液相色谱-串联质谱法测定水产品中麻醉剂3-氨基苯甲酸乙酯甲基磺酸盐(MS-222)残留量的方法。提取液为50%的甲醇及乙酸-乙酸钠缓冲溶液,提取液经C18固相萃取柱净化处理后用液相色谱-串联质谱仪进行测定,外标法定量。流动相为0.5%的甲酸溶液和乙腈(V:V=60:40),流速为0.2 mL/min。该方法的线性范围为0.001~1.0 mg/L,相关系数大于0.999,检出限为1μg/kg,定量限为2μg/kg。加标回收率可以达到80%~110%。 相似文献
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Process reinforcement research was carried out in Y‐junction slug flow microreactors under variable conditions, using EHEHPA (2‐ethylhexyl phosphonic acid mono‐2‐ethylhexyl) to extract yttrium(III) from hydrochloric acid solution. The influence of pH and flow rate on the extraction‐reaction efficiency, slug size, mass transfer performance was assessed. The experimental results showed that maximum extraction‐reaction efficiency of 91.85% can be achieved in the smallest microreactor (residence time is 11.25 s), which was significantly higher than traditional extraction requiring more than 10 min. The slug length tended to decrease with the increase of pH and flow rate. Volumetric mass transfer coefficients for the slug flow microreactors were found to be in the range of 1.39×10?1—1.642 s?1 that is several orders of magnitude higher as compared to traditional extractors, which testified the beneficial effects of Y‐junction slug flow microreactor. Significant mass transfer reinforcement has prompted the use of microreactor as a suitable alternative to traditional extractors, which can advantageously improve the economic and environmental development of mineral processing. 相似文献
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Amereih S Meisel T Kahr E Wegscheider W 《Analytical and bioanalytical chemistry》2005,383(7-8):1052-1059
Speciation analysis of Sb(III) and Sb(V) in a soil sample was performed through extraction and on-line isotope dilution concentration
determination after a chromatographic separation. The total Sb concentration found in a through traffic contaminated soil
sample was (4.17 μg g−1, 0.3 μg g−1 SD, n=6). It was determined using ICP-MS after soil digestion using the sodium peroxide sintering method. The optimized extraction
procedure for speciation analysis was carried out using 100 mmol L−1 citric acid at pH 2.08 by applying an ultrasonic bath for 45 min at room temperature. The effects of citric acid concentration
(0–500 mmol L−1), pH (1–6), and temperature (30–60°C) on inorganic antimony species distribution in the examined sample were studied and
optimized. The separation of Sb(III) and Sb(V) was achieved using an anion exchange column (PRP-X100) and 10 mmol L−1 EDTA and 1 mmol L−1 phthalic acid at pH 4.5 as a mobile phase. The eluent from the HPLC was mixed with an enriched (94.2%) 123Sb spike solution that was pumped by a peristaltic pump with a constant flow rate (0.5 mL min−1) in a three-way valve. The blend passed directly to the Conikal nebulizer of the ICP-MS. By using the above extraction procedure
and methodology, 43.2% Sb(V) (2.9% RSD, n=3) and 6.0% Sb(III) (1.3% RSD, n=3) of total Sb found in the sample could be detected. The detection limits achieved by the proposed method were 20 ng L−1 and 65 ng L−1 for Sb(V) and Sb(III), respectively. The precision, evaluated by using RSD with 100 ng L−1 calibration solutions, was 2.7% and 3.2% (n=6) for Sb(V) and Sb(III), respectively, in aqueous solutions. 相似文献
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Daryoush Afzali Mina Rouhani Fariba Fathirad Ali Mostafavi 《International journal of environmental analytical chemistry》2013,93(14-15):1452-1462
In the present study, multiwalled carbon nanotubes (MWCNTs) as solid phase extraction sorbent were developed for preconcentration of arsenic(V) species prior to graphite furnace atomic absorption spectrometry (GFAAS) determination. Arsenic(V) was selectively sorbed on the packed column with MWCNTs within a pH 9.5 in the presence of 2-(5-bromo-2-pyridylazo)-5-diethyl amino phenol (5-Br-PADAP). The adsorbed species was then desorbed with 1 mL of 2.0 M HNO3. Experimental parameters including pH, sample volume and flow rate, type, volume and concentration of eluent that influence the recovery of the arsenic(V) species were optimised. Under the optimised conditions, the calibration curve was linear in the range of 0.2–10.0 µg L?1 with detection limit of 0.016 µg L?1. The relative standard deviations (RSD) for seven replicate determinations at 1.0 µg L?1 level of arsenic was 6.69%. The proposed method was successfully applied to the determination of arsenic in water samples and certified reference material (NIST RSM 1643e). 相似文献
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A supported liquid membrane (SLM) technique was investigated to extract and preconcentrate Mn(II) from water, milk and blood serum. Di-2-ethylhexyl phosphoric acid (DEHPA) with kerosene as diluent was used as a carrier in the membrane to transport Mn(II) from the donor side to acceptor side. The membrane was modified with tri-n-octylphosphine oxide (TOPO) to increase its polarity. Various parameters were investigated to optimise the extraction efficiency: pH of the donor and acceptor phase, dilution factor, donor flow rate. Scanning electron microscope images of the membranes revealed that some matrix compounds were deposited on the surface, thus limiting the extraction process. The optimum conditions found were: pH 3 in the donor phase, 0.2 M nitric acid in the acceptor phase, donor flow rate between 1.0 and 0.3 ml min−1, 15% (w/v) DEPHA and 10% TOPO in kerosene as a carrier in membrane, and dilution factors of 20 times for blood serum and 30 times for milk. The extraction efficiencies were found to be low but constant and highly reproducible showing, strong dependence on sample matrix. The new SLM extraction probe was developed and optimised for Mn(II) extraction. Compared to traditional SLM configurations, this is the simplest configuration. The use of stirring allows the same sample to be extracted many times giving higher extraction efficiency and to minimise the sample size. Adsorptive stripping voltammetry (AdSV) was applied to measure Mn(II) concentration. The optimised method was used to determine the concentration of Mn(II) in water, milk and blood serum samples. 相似文献