共查询到20条相似文献,搜索用时 15 毫秒
1.
《Analytical letters》2012,45(17):2083-2089
Abstract A high-performance liquid chromatographic procedure for the determination of pirenzepine dihydrochloride as a bulk material and in its tablet dosage form (GastrozepinR) is presented. Normal phase liquid chromatography has been performed on a Micro-pack Si-10 column using ammonium hydroxide (28–30% NH3) in methanol (0.75: 99.25% v/v) as mobile phase at a flow rate of 2 ml/min. Clobazam has been used as internal standard with retention times of 1.9 and 2.8 minutes for clobazam and pirenzepine dihydrochloride, respectively at 254 nm. Analytical calibration yields a linear relationship between 5 and 25 μg/ml, with correlation coefficient of 0.999. Tablets each labelled to contain 25 mg pirenzepine dihydrochloride give mean percentage found of 99.98 ± 0.4. A plot of logarithm of concentration against time for a solution in 6 N hydrochloric acid gives a straight line with a slope of - 0.197 day?1. The proposed method is, therefore, a stability indicating method. 相似文献
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《Analytical letters》2012,45(11):2044-2057
Abstract High performance liquid chromatographic (HPLC) and UV derivative spectrophotometric (UVDS) methods were developed and validated for the quantitative determination of sotalol hydrochloride in tablets. The HPLC method was performed on a C18 column with fluorescence detection. The excitation and emission wavelengths were 235 and 310 nm, respectively. The mobile phase was composed of acetonitrile-water containing 0.1% trietylamine (7:93 v/v) and pH adjusted to 4.6 with formic acid. The UVDS method was performed taking a signal at 239.1 nm in the first derivative. The correlation coefficients (r) obtained were 0.9998 and 0.9997 for HPLC and UVDS methods, respectively. The proposed methods are simple and adaptable to routine analysis. 相似文献
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《Analytical letters》2012,45(15):2985-3002
Abstract A simplified high performance liquid chromatographic method was developed to determine the levels of nifedipine in human plasma. Nifedipine and the internal standard, 11-ketoprogesterone, are extracted from alkalinized plasma into organic solvent. The organic solvent is then evaporated to total dryness and the analytes are reconstituted with mobile phase and chromatographed. The limit of quantitation is 10 ng/ml using a 1.0 ml plasma sample. 相似文献
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《Analytical letters》2012,45(13):957-968
Abstract Volatile and non-volatile nitrosamines are determined at subparts per million levels in a continuous, inexpensive, low-temperature procedure when samples are compatible with the aqueous-alcoholic solvents. Individual nitrosamines are resolved by gradient elution on appropriate HPLC columns, converted to nitrite ion by ultra-violet light, combined with modified Griess reagent and the red-colored product measured at 540 nanometers. Inorganic nitrite may be determined and two, organic compounds are known to interfere. The detection level for N-nitrosodimethyl amine is 0.1 parts per million. 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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《Analytical letters》2012,45(13):1657-1669
Abstract A high performance liquid chromatographic method for the determination of tropatepine in human plasma and urines is described here. After addition of an internal standard (2 chloro-11-(4-methyl piprazine 1-yl) dibenzo (b-f)(1–4) thiazepine) to the biological fluid and extraction at pH 12.0 in hexane, the analysis was performed on a reversed phase column (C18 microBondapak) with UV detection at 231 nm. The compound was eluted by a perchlorate buffer-acetonitrile mixture with a flow rate of 1.7 ml/min. The detection limit was about 25 ng/ml; reproducibility was around 7.5% for plasma concentrations below 50 ng/ml. Mass spectrometry by direct insertion probe had validated the chromatographic results. The method was successfully applied to plasma specimen collected from a healthy human volunteer following a single intravenous administration of 20 mg of tropatepine. 相似文献
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《Analytical letters》2012,45(12):2491-2500
ABSTRACT A method for the simultaneous determination of valsartan and hydrochlorothiazide in tablets is described. The procedure, based on the use of reversed-phase high-performance liquid chromatography, is linear in the concentration range 5.0-10.0 μg ml?1 for valsartan and 0.5-2.0 μg ml?1 for hydrochlorothiazide, is simple and rapid and allows accurate and precise results. The limit of detection was 1.0 μg ml?1 for valsartan and 0.05 μg ml?1 for hydrochlorothiazide. 相似文献
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离子对反相高效液相色谱法同时测定复合维生素片中4种水溶性维生素 总被引:30,自引:0,他引:30
采用离子对反相高效液相色谱法同时测定了复合维生素片中烟酰胺、维生素B1、维生素B2、维生素B6等4种水溶性维生素的含量。样品经水溶解、过滤后,以Hypersil C18化学键合硅胶为固定相,以甲醇-0.5%(体积分数)醋酸水溶液(含2.5 mmol/L己磺酸钠,pH 2.8)(体积比为18∶82)为流动相,等度洗脱,紫外检测器于280 nm波长下检测。当烟酰胺、维生素B1、维生素B2和维生素B6的质量浓度分别在25450 mg/L,590 mg/L,2.590 mg/L,595 mg/L时,其峰面积与质量浓度的线性关系良好;日内测定平均相对标准偏差(n=7)分别为1.0%,2.2%,1.8%和1.3%;日间测定相对标准偏差(n=5)分别为1.5%,3.6%,2.4%和1.7%。该方法已成功应用于复合维生素片中4种水溶性维生素的同时测定。 相似文献
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《Analytical letters》2012,45(2):377-386
Abstract An HPLC method has been developed for the determination of danazol in human plasma. the chromatographic conditions consisted of an ODS column 80 × 7.0 mm, 3 μm; a mobile phase of 71:29, methanol:20 mM potassium dihydrogen phosphate. A UV-Visible detector was set at 288 nm to monitor the danazol peak. Danazol was extracted from plasma with acetonitrile which was salted out with potassium carbonate. Prior to salting out, cadmium sulfate was mixed with the acetonitrile-plasma mixture to remove any interfering constituents. the extracted acetonitrile layer was evaporated and the residue was reconstituted in the mobile phase before injection. the method was found to be reproducible with relative standard deviation (%rsd) from 2.3 to 7.2%. A number of clinically important drugs did not interfere with danazol determination. 相似文献
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《Analytical letters》2012,45(17-18):1793-1807
Abstract Separation by reversed-phase high performance liquid chromatography (RP-HPLC) of peptide mixtures obtained from tryptic digestion of abnormal human hemoglobins and subsequent analysis by fast atom bombardment mass spectrometry (FAB-MS) of selected peptides allow unambiguous, rapid identification of the hemoglobin variants. By this method two varied hemoglobins, Hb D Punjab and Hb J Sardegna, have been determined. The methodology described, which is simple and reliable, could be used for the detection and structural identification of known and unknown Hb variants, without amino acid (a.a.) or sequence analysis. 相似文献
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《Analytical letters》2012,45(12):2241-2252
Abstract Thiopental is an ultra-short acting barbiturate, used either to induce anesthesia, or to manage intracranial hypertension associated with head injuries. A high performance liquid chromatography method vas proposed for the rapid and easy determination of thiopental in biological fluids. After precipitation of proteins with acetonitrile the chromatographic separation vas performed onto a reversed-phase column with an acetonitrile-perchlorate buffer mixture as mobile phase. Compounds were analysed at 300nm and the detection limit vas about 0.1 mg/1. The analytical procedure vas applied to the therapeutic follow-up in patients (8 childrens. 4 adults) treated with long-term infusion of thiopental after head injury, and to a pharmacokinetic study in patients receiving a single 1Y bolus of thiopental to induce anesthesia. 相似文献
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菊花中活性成分的高效液相色谱测定与指纹图谱研究 总被引:1,自引:0,他引:1
采用高效液相色谱(HPLC)法测定了12个菊花样品中绿原酸、黄芩苷、槲皮素、木犀草素和柯因五种活性成分的含量。色谱柱为Nov-pak C18,以0.1%磷酸-甲醇为流动相,流速0.6 mL/min,梯度洗脱,检测波长为254 nm。该方法在10-3~10-5g/mL范围内线性关系良好,保留时间和峰面积相对标准偏差(RSD)分别在0.20%~0.96%、0.23%~0.77%之间,回收率在96.5%~104.0%之间。同时建立了菊花样品的指纹图谱,采用夹角余弦和相关系数法计算了12个菊花样品的相似度,并且运用MATLAB程序对相关系数法计算值进行聚类分析,结果与实际样品种属区分一致,为菊花的质量控制和种属的区分提供依据。 相似文献
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《Analytical letters》2012,45(9):1077-1085
Abstract A highly reproducible ion-pair reverse-phase high performance liquid chromatographic assay for cefmenoxime in human serum has been developed. A simple sample cleanup procedure is employed. Cefoxitin is the internal standard and separation is achieved using a C-18 μ-Bondapak column. The mobile phase consists of 20% acetonitrile and 80% 0.05 M ammonium acetate buffer containing 0.005 M tetrabutylammonium hydrogen sulphate as the ion-pair agent. Samples are quantitated by UV detector at 254 nm and 0.02 aufs with an assay sensitivity of 0.625 μg/ml. The method has been successfully applied in a clinical setting. 相似文献
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《Analytical letters》2012,45(15):2723-2731
Abstract Two procedures for separation and determination of vitamin B12 in multivitamin tablets by reversed phase high performance liquid chromatography are proposed. Sample preparation is very simple: tablets are dissolved in distilled water, centrifuged and filtered. The sample solution is directly applied in the sample loop injector and chromatograms are obtained with gradient elution using water-methanol and water-acetonitrile as solvents. The peak of vitamin B12 from samples of B-complex tablets is well separated with the two procedures. For multivitamin tablets, however, only the procedure with water and methanol as solvents was good for separation and quantification of vitamin B12. Both procedures were verified by the standard addition method and also compared to a previously developed method using electrothermal atomic absorption spectrometry for vitamin B12 determination. 相似文献
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高效液相法测定胃康片中呋喃唑酮、甘珀酸钠和盐酸小檗碱 总被引:4,自引:0,他引:4
用高效液相 (HPLC)梯度洗脱法同时测定复方胃康片中呋喃唑酮、甘珀酸钠和盐酸小檗含量。使用No va PakC18柱 ,以乙腈和 0 0 2mol/L磷酸盐缓冲溶液 (pH 7 0 )为流动相 ,3,5 二硝基苯甲酸作为内标溶液 ,使用UV检测器 ,在 2 5 4nm处对样品中上述 3种成分进行测定。测定结果表明 ,呋喃唑酮在 14 1 2mg/L~ 12 70 8mg/L、甘珀酸钠在 10 0 6mg/L~ 90 5 4mg/L、盐酸小檗碱在 99 2mg/L~ 892 8mg/L时其相对峰面积 (标准品与内标的峰面积之比 )与进样质量浓度有良好的线性关系 ,其线性相关系数分别为r =0 9997,r =0 9995和r =0 9991。 相似文献
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An RP-HPLC method for the quantitative deternunation of imazethapyr in technical product and formula-ion has been developed. Operating conditions were YWG-C18 colunmn,25cm×5.0mm i.d,methanol-water-glacial acetic acid(80 : 20: 1. 2 ,volume ratio) eluent and UV-254nm dstection.The method is reproducibieand the coefficient of variation was less than 1.5%. 相似文献
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《Analytical letters》2012,45(21-22):2183-2196
Abstract A method for the simultaneous determination of CGS 10787B and its major, metabolite (CGS 12094) in plasma is described. The two compounds, and the internal standard (dichlorinated analog), are extracted from acidified plasma with ethyl acetate, taken to dryness, and reconstituted in chromatographic mobile phase. The analytes are determined automatically by high performance liquid chromatography in the reversed-phase mode as paired ions, using [N(Bu)4]+ as the counterion. The separation of the compounds is achieved on a 3u C-8 column, with detection at 254 nm. Recovery and reproducibility assessments indicate good accuracy and precision over the range of 1.0 to 250 ug/ml for CGS 10787B and 1.0 to 100 ug/ml for CGS 12094. The method has a limit of detection of 0.2 ug/ml for both compounds, and has been shown to be adequate for studying the disposition kinetics of CGS 10787B. 相似文献