New HPLC method was developed for determination of amlodipine and valsartan in their binary mixture as a part of routine control of combined formulations. The method was validated to meet official requirements includi...New HPLC method was developed for determination of amlodipine and valsartan in their binary mixture as a part of routine control of combined formulations. The method was validated to meet official requirements including selectivity, stability, linearity, precision and accuracy. Chromatography was carried out using a LiChrospher RP-18 column, a mixture containing acetonitrile, phosphate buffer of pH 3.5 and methanol (45:45:10, v/v/v) and new fluorescence detection at 255 nm for excitation and 448 nm for emission. The effect of methanol content, pH of the buffer, flow rate, detection wavelengths and column temperature was estimated in robustness study, according to a plan defined by the Plackett-Burman design. For identification of significant effects, both graphical and statistical methods were used. Ro-bustness for dissolution test was checked estimating the effects of paddle speed, temperature and pH of dissolution medium. The method was proved to complying with all official guidelines. Therefore, it is suitable for determination of amlodipine and valsartan in their binary mixtures for different analytical and pharmaceutical purposes.展开更多
High performance liquid chromatographic method was developed valdated and applied for the simultaneous determi- nation of lisinopril and NSAIDs in bulk, pharmaceuticals formulations and human serum. A Purospher star C...High performance liquid chromatographic method was developed valdated and applied for the simultaneous determi- nation of lisinopril and NSAIDs in bulk, pharmaceuticals formulations and human serum. A Purospher star C18 (5 μm, 25 × 0.46 cm) column was used with mobile phase consisting of methanol: water: acetonitrile (80:17.5:2.5 v/v, pH 3.0) and quantitative evaluation was performed at 225 nm with a flow rate of 1.0 mL?min–1. The retention time of lisinopril was 2.2 min while naproxen, flurbiprofen, diclofenac sodium and mefenamic acid were found to be 4.0, 4.5, 5.0 and 6.7 min respectively. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the requirements laid down by International Conference on Harmonization (ICH) guidelines. The method is selective, precise, accurate and can be used for analysis of pharmaceutical preparations in quality control and clinical laboratories.展开更多
A novel stability-indicating RP-HPLC method was developed and validated for simultaneous determination of Solifenacin Succinate & Tamsulosin Hydrochloride and its impurities in tablet dosage form. The method was d...A novel stability-indicating RP-HPLC method was developed and validated for simultaneous determination of Solifenacin Succinate & Tamsulosin Hydrochloride and its impurities in tablet dosage form. The method was developed using L1 column with gradient using the mobile phase consist of solvent-A (pH = 6.6, phosphate buffer + 0.5% Triethylamine) and solvent-B (90% Acetonitrile). The eluted compounds were monitored at 225 nm. Solifenacin Succinate & Tamsulosin Hydrochloride was subjected to oxidative, acid, base, hydrolytic, thermal and photolytic stress conditions. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The limit of quantification results was ranged from 0.135 - 0.221 μg/mL for Solifenacin Succinate impurities and 0.043 - 0.090 μg/mL for Tamsulosin Hydrochloride impurities. This method is suitable for the estimation of impurities and assay of Solifenacin Succinate & Tamsulosin Hydrochloride in tablets dosage form.展开更多
A simple efficient isocratic reversed-phase HPLC method was developed and validated for the determination of clindamycin palmitate hydrochloride (CPH) and its commercially available oral solution products. Separation ...A simple efficient isocratic reversed-phase HPLC method was developed and validated for the determination of clindamycin palmitate hydrochloride (CPH) and its commercially available oral solution products. Separation was achieved on a Phenomenex Zorbax (Luna) cyano column (150 × 4.6 mm, 5 μm) with a Phenomenex cyano guard cartridge (4 × 3.0 mm) on Agilent 1050 series HPLC system. CPH and its resolution standard lincomycin were eluted isocratically at a flow rate of 1 mL/min with a simplified mobile phase (potassium phosphate buffer (5 mM, pH 3.0)—acetonitrile—tetrahydrofuran (20:75:5, v/v/v)) and detected at 210 nm. The column was maintained at 25?C. The method was validated according to USP category I requirements. Robustness and forced degradation studies were also conducted. CPH marketed drug products were obtained from a drug distributor and assayed for potency using the validated method. Validation acceptance criteria were met in all cases. The analytical range for CPH was 15 - 500 μg/mL and the linearity was r2 > 0.999 over three days. The method was determined to be specific and robust. Both accuracy (92.0% - 103.8%) and precision (0.67% - 1.52%) were established across the analytical range for low, intermediate and high QC concentrations. Method applicability was demonstrated by analyzing two marketed products of CPH, in which results showed potency >98%. The method was determined to be an enhancement over the current USP methodology for assay as a result of increased efficiency, reduced organic solvents and the elimination of matrix modifiers. This method was successfully applied for the quality assessment of: 1) currently marketed drug products and 2) will in future assess the product quality of novel dosage forms of CPH for pediatric use.展开更多
A stability-indicating RP-HPLC method has been developed and validated for simultaneous determination of Valsartan & Hydrochlorothiazide and their impurities in FDC (Fixed Dose Combination) tablet dosage form. The...A stability-indicating RP-HPLC method has been developed and validated for simultaneous determination of Valsartan & Hydrochlorothiazide and their impurities in FDC (Fixed Dose Combination) tablet dosage form. The method was developed using L1 column (250 × 4.6 mm;5 μm) with gradient elution using the mobile phase consisting of solvent-A (0.1% Ortho phosphoric acid) and solvent-B (100% Acetonitrile);the gradient program (T<sub>min</sub>/%B) was set as 0/10, 5/10, 20/60, 40/60, 41/10 and 50/10. The eluted compounds were monitored at 265 nm. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The influence of Acid, Alkaline, Oxidative, Photolytic, Thermal and Humidity stress conditions, on drug product was studied. The limit of quantification results of Valsartan, Hydrochlorothiazide and their impurities are, VAL: 0.303 μg/mL, HCTZ: 0.019 μg/mL, VAL RC-B: 0.085 μg/mL, VAL RC-C: 0.327 μg/mL, HCT RC-A: 0.017 μg/mL, CTZ: 0.080 μg/mL and 5-Chloro HCT: 0.047 μg/mL. The proposed method is suitable for the estimation of Valsartan & Hydrochlorothiazide impurities in tablets dosage form.展开更多
The present data show a fast and efficient biological sample processing method for the extraction of thiamine (vitamin B1) and its mono-(TMP) and di-(TDP) phosphate esters from hippocampus, thalamus and prefrontal cor...The present data show a fast and efficient biological sample processing method for the extraction of thiamine (vitamin B1) and its mono-(TMP) and di-(TDP) phosphate esters from hippocampus, thalamus and prefrontal cortex (PFC) and blood sample of the rodents. In addition, using the hippocampus and standards of these three compounds we validated an isocratic fluorescence HPLC procedure for a simultaneous detection of them in a single chromatogram within a total run time of about 12 min. Reproducibility for TDP, TMP and B1 was 2.66%, 4.50% and 7.43% (intraday) and 37.54%, 25.39% and 25.87% (interday), respectively. Recovery assays were between 96.0% and 101.7%. The calibration curves were linear and the concentrations of the three compounds, all in nanomolar range, were determined in the brain areas and in the blood samples. When compared to the current methods in the literature, this new method provides information on essential variables, such as linearity range and limit of detection, reproducibility and stability of thiamine, TMP and TDP in rat brain samples. The present data on sample processing and B1 and its phosphate ester level determinations are the first to be validated using hippocampus samples of rats.展开更多
Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical ...Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical method variation parameters are based on pH variability of buffer solution of mobile phase, organic ratio composition changes, stationary phase (column) manufacture, brand name and lot number variation;flow rate variation and temperature variation of chromatographic system. The analytical chemical method for assay of Atropine Sulfate conducted for robustness evaluation. The typical variation considered for mobile phase organic ratio change, change of pH, change of temperature, change of flow rate, change of column etc. Purpose: The aim of this study is to develop a cost effective, short run time and robust analytical chemical method for the assay quantification of Atropine in Pharmaceutical Ophthalmic Solution. This will help to make analytical decisions quickly for research and development scientists as well as will help with quality control product release for patient consumption. This analytical method will help to meet the market demand through quick quality control test of Atropine Ophthalmic Solution and it is very easy for maintaining (GDP) good documentation practices within the shortest period of time. Method: HPLC method has been selected for developing superior method to Compendial method. Both the compendial HPLC method and developed HPLC method was run into the same HPLC system to prove the superiority of developed method. Sensitivity, precision, reproducibility, accuracy parameters were considered for superiority of method. Mobile phase ratio change, pH of buffer solution, change of stationary phase temperature, change of flow rate and change of column were taken into consideration for robustness study of the developed method. Results: The limit of quantitation (LOQ) of developed method was much low than the compendial method. The % RSD for the six sample assay of developed method was 0.4% where the % RSD of the compendial method was 1.2%. The reproducibility between two analysts was 100.4% for developed method on the contrary the compendial method was 98.4%.展开更多
建立了一种同柱分离检测44%砜吡草唑·异丙隆悬浮剂中有效成分的高效液相色谱定量方法,确定的色谱条件为250 mm×4.6 mm ODS-C18不锈钢色谱柱和紫外检测器,柱温30℃,甲醇+水溶液(60︰40,体积比)为流动相,检测波长为220 nm。结...建立了一种同柱分离检测44%砜吡草唑·异丙隆悬浮剂中有效成分的高效液相色谱定量方法,确定的色谱条件为250 mm×4.6 mm ODS-C18不锈钢色谱柱和紫外检测器,柱温30℃,甲醇+水溶液(60︰40,体积比)为流动相,检测波长为220 nm。结果表明:在设定的质量浓度范围内,砜吡草唑和异丙隆的线性相关系数r均为0.9999,变异系数分别为1.07%和0.1421%,回收率分别为99.78%和99.50%,说明该方法操作简单、分离效果好,线性关系、准确度和精密度均符合分析的基本要求,可用于制剂产品中砜吡草唑和异丙隆的质量控制。展开更多
Saffron,the dried stigma of Crocus sativus L.,findsnumerous applications in TCM.Here,a novel HPLC protocol was established and applied for the analysis of saffron samples,not only from different places of origin but a...Saffron,the dried stigma of Crocus sativus L.,findsnumerous applications in TCM.Here,a novel HPLC protocol was established and applied for the analysis of saffron samples,not only from different places of origin but also from several harvest seasons.One of the main active constituents of saffron,crocin,is also contained in展开更多
A new method using high-performance liquid chromatography coupled with ultra violet detection(HPLC–UV)was developed and validated for the simultaneous quantification of atazanavir,dolutegravir,darunavir,efavirenz,etr...A new method using high-performance liquid chromatography coupled with ultra violet detection(HPLC–UV)was developed and validated for the simultaneous quantification of atazanavir,dolutegravir,darunavir,efavirenz,etravirine lopinavir,raltegravir,rilpivirine and tipranavir in human plasma.For the first time we reported here the development and validation of an HPLC–UV assay to quantify the frequently administered 9antiretroviral compounds including dolutegravir and rilpivirine.A simple solid phase extraction procedure was applied to 500 μL aliquots of plasma.The chromatographic separation of the drugs and internal standard(quinoxaline) was achieved with a gradient of acetonitrile and sodium acetate buffer on a C_(18) reverse-phase analytical column with a 25 min analytical run time.Calibration curves were optimised according to the therapeutic range of drug concentrations in patients,and the coefficient of determination(r^2) was higher than0.99 for all analytes.Mean intraday and interday precisions(RSD) for all compounds were less than 15.0%,and the mean accuracy(% deviation from nominal concentration) was also found to be less than 15.0%.Extraction recovery range was between 80% and 120% for all drugs analysed.The solid phase extraction and HPLC–UV method enable a specific,sensitive,and reliable simultaneous determination of nine antiretroviral agents in plasma.Good extraction efficiency and low limit of HPLC–UV quantification make this method suitable for use in clinical trials and therapeutic drug monitoring.展开更多
目的比较不同炮制条件对地骨皮化学成分的影响,优选饮片炮制方法。方法采用HPLC-IT-TOF/MS;ZORBAX SB-Aq C_(18)色谱柱;流动相为0.1%甲酸水溶液-乙腈梯度洗脱;柱温40℃;流速0.3 mL/min;进样体积5μL;电喷雾离子源(Electrospray Ionizati...目的比较不同炮制条件对地骨皮化学成分的影响,优选饮片炮制方法。方法采用HPLC-IT-TOF/MS;ZORBAX SB-Aq C_(18)色谱柱;流动相为0.1%甲酸水溶液-乙腈梯度洗脱;柱温40℃;流速0.3 mL/min;进样体积5μL;电喷雾离子源(Electrospray Ionization,ESI),正、负离子模式下扫描,根据相对分子质量和碎片离子等质谱信息,结合文献信息以及数据库鉴定化学成分,并以各成分的离子峰面积比作为不同炮制品的变化指数进行比较。根据鉴定结果将地骨皮5种主要活性成分的相对含量进行逼近理想解排序法分析(technique for order preference by similarity to ideal solution,TOPSIS),以客观评价经不同炮制方法所得地骨皮的品质。结果共鉴定23种化合物,其中亚麻酸在烘干80℃、焙干100℃时消失,甜菜碱在淘洗2次后消失。地骨皮在不同炮制方法下各成分含量差异较大,随着淘洗次数的增加,地骨皮中成分含量迅速下降;甜菜碱含量随着烘制温度的升高而升高,相反咖啡酰丁二胺含量会随着烘制温度的升高而降低;地骨皮甲素、地骨皮乙素均在50℃烘干时含量最高,绿原酸晒干时含量最高。通过对7种地骨皮样品进行综合评价分析,发现30℃晒干,淘洗1次(S1)为最佳炮制方式。结论地骨皮各炮制品中化合物种类和成分均发生变化;S1为最佳炮制方式。阐明了经不同炮制方法后地骨皮成分变化规律,并为地骨皮质量控制和评价奠定基础。展开更多
文摘New HPLC method was developed for determination of amlodipine and valsartan in their binary mixture as a part of routine control of combined formulations. The method was validated to meet official requirements including selectivity, stability, linearity, precision and accuracy. Chromatography was carried out using a LiChrospher RP-18 column, a mixture containing acetonitrile, phosphate buffer of pH 3.5 and methanol (45:45:10, v/v/v) and new fluorescence detection at 255 nm for excitation and 448 nm for emission. The effect of methanol content, pH of the buffer, flow rate, detection wavelengths and column temperature was estimated in robustness study, according to a plan defined by the Plackett-Burman design. For identification of significant effects, both graphical and statistical methods were used. Ro-bustness for dissolution test was checked estimating the effects of paddle speed, temperature and pH of dissolution medium. The method was proved to complying with all official guidelines. Therefore, it is suitable for determination of amlodipine and valsartan in their binary mixtures for different analytical and pharmaceutical purposes.
文摘High performance liquid chromatographic method was developed valdated and applied for the simultaneous determi- nation of lisinopril and NSAIDs in bulk, pharmaceuticals formulations and human serum. A Purospher star C18 (5 μm, 25 × 0.46 cm) column was used with mobile phase consisting of methanol: water: acetonitrile (80:17.5:2.5 v/v, pH 3.0) and quantitative evaluation was performed at 225 nm with a flow rate of 1.0 mL?min–1. The retention time of lisinopril was 2.2 min while naproxen, flurbiprofen, diclofenac sodium and mefenamic acid were found to be 4.0, 4.5, 5.0 and 6.7 min respectively. Suitability of this method for the quantitative determination of the drugs was proved by validation in accordance with the requirements laid down by International Conference on Harmonization (ICH) guidelines. The method is selective, precise, accurate and can be used for analysis of pharmaceutical preparations in quality control and clinical laboratories.
文摘A novel stability-indicating RP-HPLC method was developed and validated for simultaneous determination of Solifenacin Succinate & Tamsulosin Hydrochloride and its impurities in tablet dosage form. The method was developed using L1 column with gradient using the mobile phase consist of solvent-A (pH = 6.6, phosphate buffer + 0.5% Triethylamine) and solvent-B (90% Acetonitrile). The eluted compounds were monitored at 225 nm. Solifenacin Succinate & Tamsulosin Hydrochloride was subjected to oxidative, acid, base, hydrolytic, thermal and photolytic stress conditions. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The limit of quantification results was ranged from 0.135 - 0.221 μg/mL for Solifenacin Succinate impurities and 0.043 - 0.090 μg/mL for Tamsulosin Hydrochloride impurities. This method is suitable for the estimation of impurities and assay of Solifenacin Succinate & Tamsulosin Hydrochloride in tablets dosage form.
文摘A simple efficient isocratic reversed-phase HPLC method was developed and validated for the determination of clindamycin palmitate hydrochloride (CPH) and its commercially available oral solution products. Separation was achieved on a Phenomenex Zorbax (Luna) cyano column (150 × 4.6 mm, 5 μm) with a Phenomenex cyano guard cartridge (4 × 3.0 mm) on Agilent 1050 series HPLC system. CPH and its resolution standard lincomycin were eluted isocratically at a flow rate of 1 mL/min with a simplified mobile phase (potassium phosphate buffer (5 mM, pH 3.0)—acetonitrile—tetrahydrofuran (20:75:5, v/v/v)) and detected at 210 nm. The column was maintained at 25?C. The method was validated according to USP category I requirements. Robustness and forced degradation studies were also conducted. CPH marketed drug products were obtained from a drug distributor and assayed for potency using the validated method. Validation acceptance criteria were met in all cases. The analytical range for CPH was 15 - 500 μg/mL and the linearity was r2 > 0.999 over three days. The method was determined to be specific and robust. Both accuracy (92.0% - 103.8%) and precision (0.67% - 1.52%) were established across the analytical range for low, intermediate and high QC concentrations. Method applicability was demonstrated by analyzing two marketed products of CPH, in which results showed potency >98%. The method was determined to be an enhancement over the current USP methodology for assay as a result of increased efficiency, reduced organic solvents and the elimination of matrix modifiers. This method was successfully applied for the quality assessment of: 1) currently marketed drug products and 2) will in future assess the product quality of novel dosage forms of CPH for pediatric use.
文摘A stability-indicating RP-HPLC method has been developed and validated for simultaneous determination of Valsartan & Hydrochlorothiazide and their impurities in FDC (Fixed Dose Combination) tablet dosage form. The method was developed using L1 column (250 × 4.6 mm;5 μm) with gradient elution using the mobile phase consisting of solvent-A (0.1% Ortho phosphoric acid) and solvent-B (100% Acetonitrile);the gradient program (T<sub>min</sub>/%B) was set as 0/10, 5/10, 20/60, 40/60, 41/10 and 50/10. The eluted compounds were monitored at 265 nm. The developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantitation, accuracy, precision and robustness. The influence of Acid, Alkaline, Oxidative, Photolytic, Thermal and Humidity stress conditions, on drug product was studied. The limit of quantification results of Valsartan, Hydrochlorothiazide and their impurities are, VAL: 0.303 μg/mL, HCTZ: 0.019 μg/mL, VAL RC-B: 0.085 μg/mL, VAL RC-C: 0.327 μg/mL, HCT RC-A: 0.017 μg/mL, CTZ: 0.080 μg/mL and 5-Chloro HCT: 0.047 μg/mL. The proposed method is suitable for the estimation of Valsartan & Hydrochlorothiazide impurities in tablets dosage form.
文摘The present data show a fast and efficient biological sample processing method for the extraction of thiamine (vitamin B1) and its mono-(TMP) and di-(TDP) phosphate esters from hippocampus, thalamus and prefrontal cortex (PFC) and blood sample of the rodents. In addition, using the hippocampus and standards of these three compounds we validated an isocratic fluorescence HPLC procedure for a simultaneous detection of them in a single chromatogram within a total run time of about 12 min. Reproducibility for TDP, TMP and B1 was 2.66%, 4.50% and 7.43% (intraday) and 37.54%, 25.39% and 25.87% (interday), respectively. Recovery assays were between 96.0% and 101.7%. The calibration curves were linear and the concentrations of the three compounds, all in nanomolar range, were determined in the brain areas and in the blood samples. When compared to the current methods in the literature, this new method provides information on essential variables, such as linearity range and limit of detection, reproducibility and stability of thiamine, TMP and TDP in rat brain samples. The present data on sample processing and B1 and its phosphate ester level determinations are the first to be validated using hippocampus samples of rats.
文摘Background: The robustness is a measurement of an analytical chemical method and its ability to contain unaffected by little with deliberate variation of analytical chemical method parameters. The analytical chemical method variation parameters are based on pH variability of buffer solution of mobile phase, organic ratio composition changes, stationary phase (column) manufacture, brand name and lot number variation;flow rate variation and temperature variation of chromatographic system. The analytical chemical method for assay of Atropine Sulfate conducted for robustness evaluation. The typical variation considered for mobile phase organic ratio change, change of pH, change of temperature, change of flow rate, change of column etc. Purpose: The aim of this study is to develop a cost effective, short run time and robust analytical chemical method for the assay quantification of Atropine in Pharmaceutical Ophthalmic Solution. This will help to make analytical decisions quickly for research and development scientists as well as will help with quality control product release for patient consumption. This analytical method will help to meet the market demand through quick quality control test of Atropine Ophthalmic Solution and it is very easy for maintaining (GDP) good documentation practices within the shortest period of time. Method: HPLC method has been selected for developing superior method to Compendial method. Both the compendial HPLC method and developed HPLC method was run into the same HPLC system to prove the superiority of developed method. Sensitivity, precision, reproducibility, accuracy parameters were considered for superiority of method. Mobile phase ratio change, pH of buffer solution, change of stationary phase temperature, change of flow rate and change of column were taken into consideration for robustness study of the developed method. Results: The limit of quantitation (LOQ) of developed method was much low than the compendial method. The % RSD for the six sample assay of developed method was 0.4% where the % RSD of the compendial method was 1.2%. The reproducibility between two analysts was 100.4% for developed method on the contrary the compendial method was 98.4%.
文摘建立了一种同柱分离检测44%砜吡草唑·异丙隆悬浮剂中有效成分的高效液相色谱定量方法,确定的色谱条件为250 mm×4.6 mm ODS-C18不锈钢色谱柱和紫外检测器,柱温30℃,甲醇+水溶液(60︰40,体积比)为流动相,检测波长为220 nm。结果表明:在设定的质量浓度范围内,砜吡草唑和异丙隆的线性相关系数r均为0.9999,变异系数分别为1.07%和0.1421%,回收率分别为99.78%和99.50%,说明该方法操作简单、分离效果好,线性关系、准确度和精密度均符合分析的基本要求,可用于制剂产品中砜吡草唑和异丙隆的质量控制。
文摘Saffron,the dried stigma of Crocus sativus L.,findsnumerous applications in TCM.Here,a novel HPLC protocol was established and applied for the analysis of saffron samples,not only from different places of origin but also from several harvest seasons.One of the main active constituents of saffron,crocin,is also contained in
基金supported by “Ministero della Salute” “Ricerca corrente 2015” grant to E.C.
文摘A new method using high-performance liquid chromatography coupled with ultra violet detection(HPLC–UV)was developed and validated for the simultaneous quantification of atazanavir,dolutegravir,darunavir,efavirenz,etravirine lopinavir,raltegravir,rilpivirine and tipranavir in human plasma.For the first time we reported here the development and validation of an HPLC–UV assay to quantify the frequently administered 9antiretroviral compounds including dolutegravir and rilpivirine.A simple solid phase extraction procedure was applied to 500 μL aliquots of plasma.The chromatographic separation of the drugs and internal standard(quinoxaline) was achieved with a gradient of acetonitrile and sodium acetate buffer on a C_(18) reverse-phase analytical column with a 25 min analytical run time.Calibration curves were optimised according to the therapeutic range of drug concentrations in patients,and the coefficient of determination(r^2) was higher than0.99 for all analytes.Mean intraday and interday precisions(RSD) for all compounds were less than 15.0%,and the mean accuracy(% deviation from nominal concentration) was also found to be less than 15.0%.Extraction recovery range was between 80% and 120% for all drugs analysed.The solid phase extraction and HPLC–UV method enable a specific,sensitive,and reliable simultaneous determination of nine antiretroviral agents in plasma.Good extraction efficiency and low limit of HPLC–UV quantification make this method suitable for use in clinical trials and therapeutic drug monitoring.
文摘目的比较不同炮制条件对地骨皮化学成分的影响,优选饮片炮制方法。方法采用HPLC-IT-TOF/MS;ZORBAX SB-Aq C_(18)色谱柱;流动相为0.1%甲酸水溶液-乙腈梯度洗脱;柱温40℃;流速0.3 mL/min;进样体积5μL;电喷雾离子源(Electrospray Ionization,ESI),正、负离子模式下扫描,根据相对分子质量和碎片离子等质谱信息,结合文献信息以及数据库鉴定化学成分,并以各成分的离子峰面积比作为不同炮制品的变化指数进行比较。根据鉴定结果将地骨皮5种主要活性成分的相对含量进行逼近理想解排序法分析(technique for order preference by similarity to ideal solution,TOPSIS),以客观评价经不同炮制方法所得地骨皮的品质。结果共鉴定23种化合物,其中亚麻酸在烘干80℃、焙干100℃时消失,甜菜碱在淘洗2次后消失。地骨皮在不同炮制方法下各成分含量差异较大,随着淘洗次数的增加,地骨皮中成分含量迅速下降;甜菜碱含量随着烘制温度的升高而升高,相反咖啡酰丁二胺含量会随着烘制温度的升高而降低;地骨皮甲素、地骨皮乙素均在50℃烘干时含量最高,绿原酸晒干时含量最高。通过对7种地骨皮样品进行综合评价分析,发现30℃晒干,淘洗1次(S1)为最佳炮制方式。结论地骨皮各炮制品中化合物种类和成分均发生变化;S1为最佳炮制方式。阐明了经不同炮制方法后地骨皮成分变化规律,并为地骨皮质量控制和评价奠定基础。