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VALIDATION OF A SIMPLES METHOD FOR SIMULTANEOUS DETERMINATION OF LIPOIC ACID AND RESVERATROL BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY 高效液相色谱法同时测定硫辛酸和白藜芦醇的方法验证
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.82578
I. Guerreiro, Samuel Davies, S. Guterres, S. Berlitz
A high-performance liquid chromatography-ultraviolet (HPLC-UV) method was developed and validated for simultaneous determination of Resveratrol (RSV) and Lipoic Acid (LA). A C18 column was used with a mobile phase consisting of acetonitrile and 0.01M phosphoric acid (60:40). The detection wavelength was at 235 nm. The method was specific in the presence of pharmaceutical excipients widely used in solid dosage forms or lipid-core nanocapsules. The results demonstrated linearity between 5 and 50 µg/mL for RSV and 30 and 120 µg/mL for LA. The method presented precision and accuracy (RSD <5%). In addition, the developed method was considered robust. Therefore, the developed method can be applied successfully for simultaneous determination of RSV and LA in the proposed conditions, with a potential application to assay both drugs in several dosage forms.
建立了高效液相色谱-紫外(HPLC-UV)同时测定白藜芦醇(RSV)和硫辛酸(LA)的方法。色谱柱为C18,流动相为乙腈- 0.01M磷酸(60:40)。检测波长为235 nm。该方法对广泛用于固体剂型或脂核纳米胶囊的药物赋形剂具有特异性。结果表明,RSV在5 ~ 50µg/mL之间呈线性,LA在30 ~ 120µg/mL之间呈线性。方法精密度高,准确度高(RSD <5%)。此外,该方法具有鲁棒性。因此,所建立的方法可以成功地应用于RSV和LA的同时检测,并有可能应用于多种剂型的两种药物的检测。
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引用次数: 1
LC-MS/MS METHOD FOR THE SIMULTANEOUS DETERMINATION OF CEFEPIME AND TAZOBACTAM IN DOG PLASMA Lc-ms / ms法同时测定狗血浆中头孢吡肟和他唑巴坦的含量
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.84357
K. Patil, Sukanta K. Naik, Vineet S. Zope, R. Chavan, R. Yeole
A high performance liquid chromatography (HPLC) method with tandem mass spectrometric detection (MS/MS) has been developed and validated for the simultaneous quantification of cefepime and tazobactam in dog plasma. The method was developed on amide column with isocratic elution. The developed method is simple and economic in terms of sample preparation. The method is specific, sensitive, accurate, precise and robust. The method was successfully applied for pre-clinical pharmaco-kinetic studies in dogs. The Tmax was found to be 0.5 hr, the mean Cmax and AUC(0-12) displayed dose proportionate response.
建立了同时测定狗血浆中头孢吡肟和他唑巴坦含量的高效液相色谱-串联质谱检测(MS/MS)方法。该方法采用酰胺柱等密度洗脱法。该方法在样品制备方面简便、经济。该方法具有专属性强、灵敏度高、准确度高、精密度大、鲁棒性好等特点。该方法已成功应用于犬的临床前药物动力学研究。Tmax为0.5 hr,平均Cmax和AUC(0-12)呈剂量正比反应。
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引用次数: 4
FEASIBILITY STUDY FOR ANTISEPTIC GEL FORMULATIONS INCORPORATING THE ESSENTIAL OILS CYMBOPOGON CITRATUS (DC.) STAPF. AND CARYOPHYLLUS AROMATICUS L. 含香茅精油的防腐凝胶制剂的可行性研究STAPF。和香石竹。
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.77118
L. Vinciguerra, C. Rohr, Graziela Heberlé
Recent years have seen an increase in the search by the pharmaceutical industry for products and active ingredients of natural origin. Additionally, there is a need for the creation of new market products such as antiseptics, used to prevent or reduce the risk of infection by inhibiting the proliferation of microorganisms. The objective of this study was to produce two antiseptic gels by incorporating into each of them individually an essential oil, namely lemongrass and cloves, and subsequently evaluating the antimicrobial activity by minimum inhibitory concentration (MIC) testing. The oils and gels were tested in parallel and resulted in a similar profile that can be observed in the inhibition concentration. This was a preliminary study that merits further investigation, which may progress to stability testing and evaluation of lower concentrations incorporated into the gel base.
近年来,制药行业对天然来源的产品和活性成分的研究有所增加。此外,有必要创造新的市场产品,如防腐剂,用于通过抑制微生物的增殖来预防或减少感染的风险。本研究的目的是将香茅精油和丁香精油分别掺入两种抗菌凝胶中,然后通过最低抑菌浓度(MIC)测试评估其抗菌活性。油和凝胶平行测试,结果在抑制浓度上可以观察到相似的轮廓。这是一项值得进一步研究的初步研究,可能会进行稳定性测试和低浓度凝胶基的评估。
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引用次数: 1
ANALYTICAL METHOD BY LIQUID CHROMATOGRAPHY TO ASSAY PIPERINE ASSOCIATED IN NANOEMULSIONS 液相色谱法测定纳米乳中胡椒碱的含量
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.80366
M. Motta, A. Schneider, C. Codevilla, C. R. Menezes, C. B. Silva
This work aimed to develop and validate a simple, fast and low cost analytical method for the quantification of the bioactive piperine in nanoemulsions by high performance liquid chromatography with UV detection. Nanoemulsions were prepared by spontaneous emulsification and their physicochemical properties were evaluated. Considering the chromatographic conditions, the mobile phase was composed by methanol:water (70:30, v/v), Gemini® C18 column, and UV detection at 343 nm. The method was linear in the concentration range of 5-50 μg mL-1 (r = 0.9999), specific, precise (repeatability of RSD 0.38 % and intermediate precision of RSD 1.11 %), accurate (101.3 %) and robust. Nanoemulsions showed nanometric droplet size, polidispersity index below 0.11 and negative zeta potential. The piperine content in the samples was 0.99 ± 0.01 mg mL-1. Regarding these features, the analytical conditions proposed in this work were adequate and effective to determine the piperine content in nanoemulsions.
本研究旨在建立一种简单、快速、低成本的紫外检测高效液相色谱法定量测定纳米乳中辣椒碱的方法。采用自发乳化法制备了纳米乳液,并对其理化性质进行了评价。考虑色谱条件,流动相为甲醇:水(70:30,v/v), Gemini®C18色谱柱,343 nm紫外检测。该方法在5 ~ 50 μ mL-1的浓度范围内呈良好的线性关系(r = 0.9999),具有专属性、精密度(重复性RSD为0.38%,中间精密度RSD为1.11%)、准确度(101.3%)和鲁棒性。纳米乳液的微滴尺寸为纳米级,多分散度指数小于0.11,zeta电位为负。样品中胡椒碱含量为0.99±0.01 mg mL-1。考虑到这些特点,本文提出的分析条件对纳米乳中胡椒碱含量的测定是充分和有效的。
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引用次数: 1
SECOND-ORDER DERIVATIVE UV SPECTROPHOTOMETRIC AND RP-HPLC METHODS FOR THE ANALYSIS OF VILDAGLIPTIN AND APPLICATION FOR DISSOLUTION STUDY 二阶导数紫外分光光度法和反相高效液相色谱法分析维格列汀及其溶出度研究
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.86511
A. Barden, B. Piccoli, N. Volpato, M. Steppe
This study describes two analytical methods, by second-order derivative UV spectrophotometric by HPLC, for determination of vildagliptin, a drug used for treatment of type 2 Diabetes Mellitus that belongs to a therapeutic class called inhibitors of dipeptidyl peptidase 4. The methods were validated in accordance with ICH and USP requirements. Analyses by UV derivative method were performed at 220 nm, which was the zero crossing point of excipient solutions. HPLC was optimized and the analysis was carried out using a Zorbax Eclipse Plus RP-C8 column (150 mm × 4.6 mm, 5 μm), detection at 207 nm, and potassium phosphate buffer solution pH 7.0 : acetonitrile (85:15, v/v) as mobile phase. In dissolution test, the conditions used were 0.01 mol L-1 hydrochloric acid in 900 mL of dissolution medium, USP apparatus 2 (paddle) and 50 rpm stirring speed. Both methods were successfully applied for analysis of dissolution samples from marketed vildagliptin tablets.
维格列汀是一种用于治疗2型糖尿病的药物,属于二肽基肽酶4抑制剂,本研究描述了用高效液相色谱法二阶导数紫外分光光度测定维格列汀的两种分析方法。方法按照ICH和USP的要求进行了验证。用紫外导数法在220 nm处进行分析,220 nm为赋形剂溶液的零交叉点。HPLC优化,色谱柱为Zorbax Eclipse Plus RP-C8 (150 mm × 4.6 mm, 5 μm),检测波长为207 nm,流动相为磷酸钾缓冲液pH 7.0:乙腈(85:15,v/v)。溶出试验条件为:盐酸浓度为0.01 mol L-1,溶解介质为900 mL, USP装置2(桨叶),搅拌速度为50 rpm。两种方法均可用于市售维格列汀片溶出度分析。
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引用次数: 4
DEVELOPMENT AND VALIDATION OF A SIMPLE AND FAST METHOD FOR SULFONAMIDES, TETRACYCLINES AND MACROLIDES IN HONEY USING LC-MS/MS lc-ms / ms快速测定蜂蜜中磺胺类、四环素类和大环内酯类物质的方法的建立与验证
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.84248
Cristina Ribeiro, M. T. Martins, L. Jank, F. Barreto, R. Hoff, J. Arsand
Antibacterial are widely used in veterinary applications for diseases treatment and prophilatic purposes. Inadequate uses of these drugs can lead of undesirable residues in honey for consumption. In Brazil, the legal authorities set a maximum residue limit (MRL) for different compound in honey, ranging from 10 to 20 ng ml-1. The monitoring of antibacterials is a concern, since it constitutes a risk to human health and collaborates with the growth of resistant bacteria. Brazil has the National Residue Control Plan (NRCP) to ensure that the products traded are compliant with the safety and quality criteria required by consumers. The goal of this work was to develop and validate a method suitable to determine sulfonamides, tetracyclines and macrolides in honey, using liquid chromatography tandem mass spectrometry. The main objective was to develop an efficient technique, combining simplicity, speed and low cost, since the method will be employed in routine analysis. Recoveries between 36 to 139% were obtained. Good linearity (r2) above 0.95, considering three different days, for all drugs was achieved in concentrations ranging from 0 to 200% of the MRL. Intraday and inter-day precision with CV% (n=6) lower than 18%, in agreement with specifications were obtained in concentrations ranging from 0.5 to 1.5 MRL, except for erythromycin. Accuracy was between 97 to 108%. Limits of quantitation for macrolides were 2.5 ng g-1and for sulfonamides and tetracyclines were 5 ng g-1. Decision limit (CCα) was evaluated and the results obtained were between 12.9 to 28.1 ng g-1. The detection capability (CCβ) obtained was between 15.8 to 36.3 ng g-1. The proposed method demonstrated to be suitable for this intended purpose and will contribute to antibacterial honey monitoring.
抗菌药物广泛应用于兽医疾病治疗和生殖目的。这些药物的使用不当会导致蜂蜜中的不良残留物。在巴西,法律当局为蜂蜜中的不同化合物设定了最大残留限量(MRL),范围为10至20 ng ml-1。对抗菌素的监测是一个令人关切的问题,因为它对人类健康构成风险,并与耐药细菌的生长相辅相成。巴西有国家残留控制计划(NRCP),以确保交易的产品符合消费者要求的安全和质量标准。本工作的目的是建立并验证一种适用于测定蜂蜜中磺胺类、四环素类和大环内酯类的液相色谱串联质谱法。主要目标是开发一种高效的技术,结合简单,快速和低成本,因为该方法将用于常规分析。加样回收率为36 ~ 139%。考虑到三个不同的天数,所有药物的浓度在0到200%的MRL范围内均达到良好的线性(r2),高于0.95。除红霉素外,日内日内精密度CV% (n=6)低于18%,符合标准,浓度范围为0.5 ~ 1.5 MRL。准确率在97 - 108%之间。大环内酯类的定量限为2.5 ng g-1,磺胺类和四环素类的定量限为5 ng g-1。评价决策限(CCα),结果在12.9 ~ 28.1 ng g-1之间。所得的检测能力(CCβ)在15.8 ~ 36.3 ng g-1之间。所提出的方法被证明适合于这一预期目的,并将有助于抗菌蜂蜜的监测。
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引用次数: 5
MICROBIOLOGICAL ASSAY FOR THE DETERMINATION OF CEFPIROME IN RAW MATERIAL AND INJECTABLE PREPARATION 原料和注射制剂中头孢匹罗的微生物测定方法
Pub Date : 2018-09-14 DOI: 10.22456/2527-2616.84473
T. P. Oppe, Júlia Menegola, E. Schapoval
Cefpirome is a fourth-generation cephalosporin active against a broad spectrum of gram-negative and gram-positive bacterial infections. The present work describe the development and validation of a simple, sensitive and specific agar diffusion bioassay applying cylinder-plate method for quantification of cefpirome in raw material and powder for injectable preparation. The validation method yielded good results and included linearity, precision, accuracy and specificity. The assay is based on the inhibitory effect of cefpirome upon the strain of Kocuria rizophila ATCC 9341 as the test microorganism. The result of assay were treated statistically by ANOVA and the response graphs for standard and sample solutions were linear (r = 0.9948) in the range of 0.3 – 1.2 µg mL-1, precise (intra-assay: RSD = 0.11; inter-assay: RSD = 0.18) and accurate (mean recovery value = 99.41%). A preliminary stability study of cefpirome showed that the microbiological assay is specific for the determination cefpirome in the presence of its degradation products. The proposed microbiological method allows the quantitation of cefpirome in pharmaceutical dosage form and raw material and can be used for the drug analysis in routine quality control.
头孢匹罗是抗广谱革兰氏阴性和革兰氏阳性细菌感染的第四代头孢菌素。本文描述了一种简单、灵敏、特异的琼脂扩散生物测定方法的建立和验证,该方法应用圆筒-平板法定量注射制剂原料和粉末中的头孢匹罗。验证方法具有良好的线性度、精密度、准确度和特异性。本实验以头孢匹罗为试验微生物,考察其对嗜枯病菌ATCC 9341的抑制作用。分析结果采用方差分析进行统计学处理,标准溶液和样品溶液的响应图在0.3 ~ 1.2µg mL-1范围内呈线性关系(r = 0.9948),精确(测定内:RSD = 0.11;测定间:RSD = 0.18),准确度高(平均回收率= 99.41%)。头孢匹罗的初步稳定性研究表明,微生物测定法对存在降解产物的头孢匹罗的测定具有特异性。该方法可用于头孢匹罗制剂剂型和原料的定量,可用于常规质量控制中的药物分析。
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引用次数: 5
Simultaneous analysis of dapagliflozin and its three related impurities by stability-indicating UPLC method and in vitro toxicity evaluation 稳定性指示UPLC法同时分析达格列净及其3种相关杂质及体外毒性评价
Pub Date : 2008-08-21 DOI: 10.22456/2527-2616.128661
L. Bueno, J. W. Manoel, M. Koetz, A. Henriques, M. Steppe, E. Schapoval
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引用次数: 0
期刊
Drug Analytical Research
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