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5—氨基水杨酸锌及相关物质的高效毛细管电泳分离与测定 总被引:2,自引:0,他引:2
1引言5-氨基水杨酸是治疗胃溃疡和Crohn疾病的药物。为提高稳定性和药物疗效,最近合成了新药物5-氨基水杨酸锌。我们对5-氨基水杨酸锌与主要杂质水杨酸,以及可能降解产物5-氢基水杨酸与对氨基苯酚等物质的高效毛细管电泳(HPCE)的分离与测定进行了研究,结果表明,本法分离效果好,测定准确,具有较好的应用价值。2实验部分1229HPCEANALYSER(北京新技术应用研究所),石英毛细管(65.5cm×50μmi.d,有效长度57.3cm,河北永年光纤厂)。5-氨基水杨酸锌(ZnASA,99%),… 相似文献
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作者以新研制的4-(6-甲基-2-苯并噻唑偶氨)间苯三酚为柱前衍生试剂,用含10mmol/L的pH6.80的HAc-NaAc缓冲溶液,10mmol/LTBA·Br和1×10 ̄(-4)mol/LEDTA的甲醇-水溶液(78:22,V/V)作流动相,在C_(18)柱上,11min内反相HPLC分离测定了Cr(Ⅵ),V(Ⅴ)Co(Ⅱ),Ni(Ⅲ)。当S/N=3时,其检出限分别是V(Ⅴ)5.45ng,Co(Ⅱ)1.09ng,Ni(Ⅱ)1.50ng,Cr(Ⅵ)1.70ng。 相似文献
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反相HPLC测定钒,铌,钽的2—(2—吡啶偶氮)—5—二乙氨基苯酚配合物 总被引:1,自引:0,他引:1
以2-(2-吡啶偶氮0-5-二乙氨基苯酚(PADAP)为柱前衍生试剂,在含0.1%酒石酸的10mmol/L(pH3.5)HAc-NaAc缓冲溶液的甲醇/水(50∶50,V/V)中(580nm检测),在C18柱上于11min内实现了V、Nb、Ta的同时分离及测定,检出限(S/N=3)杰0.34、0.29、7.30ng/mL.该法灵敏度高,用于矿样分析所得民推荐值相行,标准加入回收率为99.0%~10 相似文献
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环己酮与硫代碳酰肼在不同介质中的反应,合成出两个不同的环己烷螺含氮杂环化合物。经X-射线结构分析确定它们分别为1,2,4,5-四氮螺[5,5]十一烷-3-硫酮,C_7H_(14)N_4S(Ⅰ)和1,2,4,-三氮螺[4,5]癸-1-烯-4-氨基-3-硫酮。C_7H_(12)N_4S_x(S_x=0.8S+0.2O)(Ⅱ)。晶体学参数分别为(Ⅰ):P2_1/c,a=12.026(4),b=26.817(6),c=12.042(3),β=115.94(2)°,Z=4,V=933.4(10),M_r=186.28;(Ⅱ):P2_1/m,a=6.595(7),b=6.817(6),c=10.572(6),β=106.3(1)°,V=456(1),Z=2,M_r=181.05。最终一致因子分别为R=0.054,R_w=0.065和R=0.089,R_w=0.096。两个化合物中,环己烷都为椅式构型,它与其螺联的6员氮杂环,5员氮杂环的最小二乘平面间的夹角分别为68.94和90°。并对合成反应途径作了初步讨论。 相似文献
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KBrO3—KBr紫外分光光度法测定痕量水杨酸 总被引:5,自引:0,他引:5
研究了HCl溶液中KBrO3-KBr紫外分光光度法测定水杨酸的条件,建立了测定痕量水杨酸的新方法。结果表明,在0.6mol/LHCl,3*10^-5mol/LKBrO3,5*10^-4mol/LKBr,6*10^-4mol/lKI溶中测定水杨酸,其线性范围为0.2-4.0mg/L,表观摩尔吸光系数为1.9*10^-4L.mol^-1.cm^-1,Sandell为7.3μg/cm^2。sg if e 相似文献
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芳族硝基化合物电还原中Cu-Ni合金的电极活性 总被引:5,自引:0,他引:5
本文采用共沉积法制备了以铜为基体的不同Cu/Ni比的Cu-Ni合金镀层,并用稳态极化法研究了这些镀层在使用硝基苯(NB)和1,5-二硝基蒽醌(1.5-DNA)制备对氨基苯酚(PAP)及1,5-二氨基-4,8-二羟基蒽醌(1,5-DA-4,8-DHA)等电化学还原过程中的阴极活性.研究表明,在PAP和1,5-DA-4,8-DHA电合成体系中,不同Cu/Ni比的合金阴极具有不同的交换电流密度(io)和表观活化能(EA),其中以0.05mol/LCuSO4·5H2O+0.6mol/LNiSO4·6H2O+0.25mol/LNa3Cit·2H2O组成的镀液,并在控制电流密度为0.6A·dm-2、pH值为6、体系温度为50℃等工艺条件下镀制的Cu-Ni合金试片(CN-30),具有最大的io和最小的EA值,与常规所用的Cu、Cu/Hg、蒙乃尔合金等阴极相比,CN-30试片的电极性能最佳 相似文献
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TPPC在0.08mol/LCH3COONa和0.4mol/LCH3COOH(NaAc-HAc下同)底液条件下,在电位-1.57V附近产生一尖锐的导数波,峰高在3.7×10^-6-5.6×10^-5mol/L范围内呈线性关系,同时,讨论了极谱波的性质及电极反应机理。 相似文献
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Błazewicz A Fijałek Z Warowna-Grześkiewicz M Boruta M 《Journal of chromatography. A》2007,1149(1):66-72
A sensitive and selective HPLC method with amperometric detection (HPLC-ED) for the determination of rocuronium bromide and its eight impurities has been developed. The analysis was performed on Hypersil 100 Silica column 5 microm (250 mm x 4.6 mm; Thermo Electron). The mobile phase consisting of 4.53 g l(-1) solution of tetramethylammonium hydroxide adjusted to pH 7.4 with 85% phosphoric acid:acetonitrile (1:9), was found the best for the separation and determination of the studied compounds. The chromatograms were recorded over 10 min using the amperometric detection at a potential +0.9 V of the glassy carbon electrode versus the reference electrode Ag/AgCl. The limit of quantitation was 45 ng ml(-1) for rocuronium and from 25 to 750 ng ml(-1) for the examined impurities. The proposed HPLC-ED method was successfully applied to the analysis of rocuronium and its impurities in Esmeron solution for injection. 相似文献
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A micellar electrokinetic chromatographic (MEKC) method was developed for the quantification of mesalazine or 5-aminosalicylic acid (5-ASA) and its major impurities 3-aminosalicylic acid, salicylic acid, sulfanilic acid and 4-aminophenol. The optimisation of the experimental conditions was carried out considering some important requirements: resolution, reproducibility, detection limits of 0.1% (m/m) or less, short total analysis time. Preliminary investigations employing sodium dodecyl sulfate (SDS) as surfactant did not lead to the necessary resolution of the studied compounds; the addition of tetrabutylammonium bromide (TBAB) to the SDS micellar system resulted in the complete separation of all the compounds. The effects on the separation by several parameters such as TBAB concentration, SDS concentration, background electrolyte pH and concentration, were evaluated. Using a fused-silica capillary (8.5 cm effective length) complete analysis was obtained in a very short time. Under the optimised final conditions [120 mM 3-(cyclohexylamino)-2-hydroxy-1-propanesulfonic acid buffer, pH 10.20, 65 mM SDS in the presence of 55 mM TBAB and 5% methanol] the method was validated for specificity, precision, linearity, limits of detection and quantitation, and robustness: the 5-ASA related impurities can be quantified at least at the 0.1% (m/m) level. 相似文献
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建立了分离测定萘普生和溴代萘普生的反相键合相高效液相色谱法。采用ODS柱,以添加50mmol/L乳酸并用高氯酸调节pH为2.5的80%甲醇-水溶液作为流动相,以苯甲酸为内标物,测定了不对称合成工艺产物中萘普生和溴代萘普生的含量。方法的准确度分别为99.83%~102.07%(萘普生)和99.0%~100.83%(溴代萘普生),相对标准偏差分别小于2.58%(萘普生)和3.64%(溴代萘普生)。方法可用于工艺条件的选择和质量检测。 相似文献
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唑来膦酸及其有关化合物的反相离子对高效液相色谱分离 总被引:6,自引:0,他引:6
采用反相离子对高效液相色谱法研究了唑来膦酸及其有关化合物的色谱分析与分离方法。优化的分离条件:以Hypersil C8柱为固定相,以甲醇-5 mmol/L磷酸二氢钠缓冲液(含6 mmol/L四丁基溴化铵溶液,用氢氧化钠溶液调节pH至7.0)(体积比为20∶80)为流动相,等度洗脱,流速为1.0 mL/min,紫外检测波长为220 nm,柱温为室温。在该色谱条件下,唑来膦酸与有关化合物(包括其合成过程中残余的原料咪唑乙酸和其他氧化分解产物)的分离良好,与保留时间最接近的杂质峰的分离度大于2.5。该方法不需进 相似文献
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Md. Umar Khan M. A. Baseer S. Ranjith Kumar M. Saravanakumar A. G. Prasannanjali P. Badarinadh Gupta 《合成通讯》2013,43(15):2241-2253
Balsalazide disodium (Colazide®) is an oral prodrug of mesalamine (5-aminosalicylic acid) and possesses anti-inflammatory properties. During the process development for balsalazide disodium, we observed eight impurities, namely des-β-alanine balsalazide, balsalazide β-alanine, balsalazide 3-isomer, decarboxy balsalazide, bis-azo salicylic acid, biphenyl-azo salicylic acid, bis-azo diacid, and bis-azo triacid. The present work describes the synthesis and characterization of these impurities. 相似文献
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《Analytical letters》2012,45(16):2525-2533
Following optimization of extraction, separation, and analytical conditions, a simple, rapid, and sensitive HPLC-UV method was developed for the simultaneous determination of seven major bioactive components in Sambucus chinensis Lindl, including chlorogenic acid, caffeic acid, p-coumaric acid, ferulic acid, kaempferol-3-O-β-D-galactopyranoside, kaempferol-3-O-β-D-glucopyran-oside, and kaempferol-3-O-(6-actyl)-β-D-galacto-pyranoside. The good chromatographic separation was performed on a Gemini C18 reversed-phase analytical column (250 mm × 4.6 mm, 5 μm) by gradient elution with acetonitrile and formate aqueous buffer (containing 0.8% formic acid, V/V) at a flow rate of 1.0 mL/min. The detection wavelength was set at 326 nm. The intra-day and inter-day precisions were evaluated with the R.S.D. values less than 4.0%. The mean recoveries of the seven compounds were in the range of 92.4%–104.8%. The method was successfully applied to determine the seven bioactive compounds in six different origins of Sambucus chinensis Lindl samples, and there was a significant variation in the contents of the seven compounds among the six samples. Therefore, this method provided a new basis of overall assessment for routine use in the quality control of Sambucus chinensis Lindl. 相似文献
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Maha M. Abdelrahman Neven M. Habib Aml A. Emam Hamada M. Mahmoud Nada S. Abdelwhab 《Biomedical chromatography : BMC》2020,34(4):e4804
Green TLC-densitometric and RP-HPLC methods were developed and validated for the determination of the active prodrug sulfasalazine (SZ), its active metabolite mesalazine (MZ) and the major active metabolite of mesalazine, N-acetyl-5-aminosalicylic acid (AS). In the developed TLC-densitometric method, chromatographic separation was carried out on TLC silica gel plates 60 F254 using a developing system consisting of ethyl acetate–methanol–ammonia solution 33% (8:2.5:0.3, by volume) and then scanning the separated bands at 215 nm using hydrochlorothiazide as an internal standard with linearity ranges of 0.4–3, 0.4–2.4 and 0.3–2 for SZ, MZ and AS, respectively. The developed RP-HPLC method depended on chromatographic separation using a C18 column with a solvent mixture of methanol–aqueous acetic acid solution (pH 5) as a mobile phase with gradient elution mode and UV scanning at 243 nm using pyrazinamide as internal standard with linearity ranges of 5–50, 5–40, and 3–20 for SZ, MZ and AS, respectively. US Food and Drug Administration guidelines were followed during validation of the methods. The greenness of the developed methods was estimated using the greenness profile and the Eco-Scale approach. Both methods passed the four quadrants of the greenness profile and had Eco-Scale score ˃75, thus they were considered to be green according to these approaches. 相似文献
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采用反相离子对高效液相色谱/蒸发光散射检测法研究了唑来膦酸及其有关物质的色谱分析与分离方法。优化了色谱条件,固定相为Hypersil C8柱,以含10 mmol/L正戊胺的5mmol/L乙酸铵缓冲液(用乙酸调节pH至7.0)-甲醇(体积比为97:3)为流动相,流速为1.0mL/min,蒸发光散射检测器检测。在该色谱条件下,唑来膦酸与其有关化合物(包括合成过程中残余的原料咪唑乙酸及分解产物亚磷酸、磷酸盐)的分离良好,唑来膦酸色谱峰与最近杂质峰的分离度大于1.5。本法简便快速,为唑来膦酸的常规分析提供了有效可靠的方法。 相似文献
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A simple and reliable ultra performance liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry method (UPLC-TOF-MS) was developed and validated for the simultaneous determination of the major bioactive constituents in Acanthopanax senticosus and its extract. The separation of five compounds was performed on a UPLC? HSS T3 column (100 mm × 2.1 mm, 1.7 μm) with gradient elution using a mobile phase consisting of 0.1% aqueous formic acid and acetonitrile containing 0.1% formic acid. All targeted compounds (syringin, chlorogenid acid, caffeic acid, eleutheroside E and isofraxidin) were baseline separated within 5.3 min in samples, which represented an approximate six-fold reduction in the analysis time in comparison to published HPLC method. Quantitation was carried out working in the V mode using the narrow widow extracted ion chromatograms (nwXICs) of each compound (extracted using a 20 mDa window). Furthermore, all calibration curves showed good linearity (r > 0.999) within the test ranges. The precision was evaluated by intra- and inter-day tests, which revealed relative standard deviation (RSD) values of less than 3.88%. The recoveries for the quantified compounds were between 96.3% and 103.7%, with RSD values below 2.89%. According to the literature, this study represents the first investigation of the simultaneous analysis of multiple components and the method can be applied to determine the amounts of the major compounds in Acanthopanax senticosus and its extract by UPLC-TOF-MS. 相似文献