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Development Green Spectrophotometric Method for Determination of Sulfamethoxazole in Pure and Pharmaceutical Formulations 绿色分光光度法测定纯制剂和制剂中磺胺甲恶唑的含量
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000584
Al-Okab Ra, Galil Msa, Ahmed N. Al‐Hakimi
Green analytical chemistry is considered as a branch of the green chemistry and the main its goal is to achieve more green analysis in quality control laboratories through different direction, such as replacing or minimizing toxic reagents and modify or replace analytical techniques or methods with safer ones. We develop a simple, accurate and sensitive spectrophotometric procedure for determination of Sulfamethoxazole (SMX) using phenoxazine (PNZ) as green analytical reagent. The method is based on oxidation in aqueous mildly acidic medium primary amine group of SMX and coupling with PNZ in the prescient iron (III) to form a stable color having maximum absorption at 520 nm. Beer's law was obeyed in the range concentration of 0.1-6 mg/l and molar absorptivity 6.105 × 104 L.mol-1.cm-1. Sandell’s sensitivity 0.003 μg.cm-2 and detection limit (DL) 0.021 ppm. The direct determination of SMX in pure form and in its pharmaceutical formulations method successfully applied with very good recoveries 98.70%-101.5%. Green spectrophotometric analytical analyses become unique when the pharmaceutical drugs reagents combine with low concentration to determinate or estimate pharmaceutical drugs.
绿色分析化学被认为是绿色化学的一个分支,其主要目标是通过不同的方向,如替换或最小化有毒试剂,修改或替换更安全的分析技术或方法,在质量控制实验室中实现更多的绿色分析。以苯恶嗪(PNZ)为绿色分析试剂,建立了一种简单、准确、灵敏的磺胺甲恶唑(SMX)的分光光度测定方法。该方法是基于SMX的伯胺基在水温和酸性介质中氧化,并与PNZ在先兆铁(III)中偶联,形成稳定的颜色,在520 nm处具有最大吸收。浓度为0.1 ~ 6 mg/l,摩尔吸光度为6.105 × 104 l .mol-1.cm-1,符合比尔定律。桑德尔灵敏度0.003 μg。cm-2,检测限(DL) 0.021 ppm。该方法可直接测定SMX的纯度及其制剂,回收率为98.70% ~ 101.5%。当药物试剂与低浓度的药物相结合,用于药物的测定或估计时,绿色分光光度法分析方法就变得独特起来。
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引用次数: 4
HPTLC and RP-HPTLC Method Development and Validation for the Estimation of Felodipine in Bulk and Pharmaceutical Formulation 非洛地平原料药和制剂中hplc和RP-HPTLC方法的建立与验证
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000599
Jain Ps, Ansari Na, Surana Sj
The aim of this work is to establish developed and validated method for the pharmaceutical analysis of Felodipine in bulk and pharmaceutical formulation by High Performance Thin Layer Chromatography HPTLC (NP) and Reverse Phase-High Performance Thin Layer Chromatography RP-HPTLC (RP). Chromatographic separation was performed on Pre-coated aluminum plates with 250 μm layer of Silica gel 60 F254 and Silica gel 60 RP-18 TLC F254S using Toluene: Methanol (8:2 v/v) and acetonitrile: water: glacial acetic acid (8:2:1 v/v/v) as a mobile phase, respectively. Scanning was carried out densitometrically at 237 nm. The Rf value of Felodipine in NP and RP were 0.40 and 0.53 and the reliability of the method was assessed by the evaluation of linearity which was found to be 300-1800 and 500-3000 ng/band with the r2 =0.998 correlation coefficient along with the accuracy of the method in terms of % recovery was found to be from 98-101 ± 1.04 % and 99-100 ± 0.47 % and the limit of detection and quantification were 11.51, 34.90 and 29.90, 90.61, respectively. The method can be used for routine analysis of Felodipine in bulk and pharmaceutical formulation.
本研究的目的是建立高效薄层色谱-HPTLC (NP)和反相高效薄层色谱- RP-HPTLC (RP)分析原料药非洛地平的方法。分别以甲苯:甲醇(8:2 v/v)和乙腈:水:冰醋酸(8:2:1 v/v/v)为流动相,在250 μm层的硅胶60 F254和硅胶60 RP-18 TLC F254S预涂铝板上进行色谱分离。在237 nm处进行密度扫描。非洛地平在NP和RP的Rf值分别为0.40和0.53,方法的可靠性评估的线性评价被发现300 - 1800和500 - 3000 ng /乐队的r2 = 0.998相关系数随着方法的准确性的%恢复被发现从100和99 - 98 - 101±1.04%±0.47%,检测和量化的极限是11.51,34.90和29.90,90.61,分别。该方法可用于非洛地平原料药和制剂的常规分析。
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引用次数: 2
Stability Indicating 1st Derivative Synchronous Spectrofluorimetric Method for the Determination of the Newly Approved Antiviral Drug Daclatasvir in Presence of Its Oxidative and Photolytic Degradation Products: Application to Tablet Dosage Form 稳定性指示一阶导数同步荧光光谱法测定新批准抗病毒药物Daclatasvir的氧化和光解降解产物:在片剂剂型中的应用
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000597
R. El-Gamal, F. Belal
A highly sensitive, simple and rapid first derivative synchronous spectrofluorimetric method was utilized for the determination of daclatasvir dihydrochloride (DCV) in presence of its oxidative and photolytic degradation products. Where synchronous 1st derivative spectrofluorimetric approach was utilized to quantitatively determine DCV at 373 nm in presence of its oxidative degradation product and at 388 nm in presence of its photolytic degradation product that is obtained by exposing DCV to UV light at 312 nm, these were the zero-crossing wavelengths of degradation products without interference. The synchronous fluorescence was scanned at Δ λ of 80 nm. The method was found to be linear across the concentration range of 0.5-5.0 ng/mL with lower detection limit of 0.090 and lower quantification limit of 0.275 ng/mL (at 373 nm) and 0.268 ng/mL (at 388 nm). The adopted approach was successfully applied to commercial tablet and the results exhibited that the derivative synchronous fluorescence spectroscopy is a stabilityindicating method, suitable for routine use within a short analysis time. The proposed method was carefully validated for linearity, accuracy, precision, specificity and robustness.
建立了一阶导数同步荧光光谱法测定盐酸daclatasvir (DCV)氧化和光解降解产物的含量,方法灵敏、简便、快速。其中同步一阶导数荧光光谱法用于在373 nm处定量测定氧化降解产物的DCV,以及在388 nm处通过将DCV暴露在312 nm的紫外光下获得的光解降解产物,这些是无干扰的降解产物的零交叉波长。在Δ λ (80 nm)处进行同步荧光扫描。该方法在0.5 ~ 5.0 ng/mL浓度范围内呈线性关系,检测下限为0.090,定量下限分别为0.275 ng/mL (373 nm)和0.268 ng/mL (388 nm)。所采用的方法成功地应用于商品片剂,结果表明,导数同步荧光光谱法是一种稳定性指示方法,适合在短时间内常规使用。对该方法进行了线性、准确度、精密度、特异性和鲁棒性验证。
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引用次数: 3
Phytochemical Analysis in the Leaves of Chamaecrista nigricans (Leguminosae) 豆科黑豆叶片的植物化学分析
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000582
T. Ac, M. Viswanathan, K. Balakrishna, A. Patra
ObjectiveIn the present study, the plant Chamaecrista nigricans (Siruavuri in Tamil) was selected to isolate, elucidate and identify the chemical constituents present in it.MethodsLeaves were collected, shade-dried, coarsely powdered using a pulvarizor, successively extracted with various solvents of increasing polarity such as hexane, chloroform and methanol using Soxhlet apparatus. Methanol leaf extract was used for isolation and identification of chemical constituents. Column chromatography (CC) and thin layer chromatography (TLC) were used for separation and purification of chemical constituents while the isolated pure compounds were identified using UV-VIS, IR, 1H and 13C NMR spectra. GC-MS analysis was carried out to identify the chemical constituents.ResultsThree anthraquinones such as emodin, chrysophanol and physcion were isolated and identified. GC-MS analysis helped to identify diisooctyl ester 1,2-benzenedicarboxylic acid, methyl ester, (Z, Z, Z)-9,12,15-octadecatrienoic acid, nitric acid nonyl ester, 4-C-methyl-myo-inositol, n-hexadecanoic acid, 2-methyl-butanoic acid, and, octadecanoic acid.ConclusionMedicinally valuable bioactive natural compounds in this plant proved its importance in drug industry for drug development against various diseases.
目的对泰米尔植物Chamaecrista nigricans (Siruavuri)进行分离、分析和鉴定。方法采集叶片,遮荫干燥,用粉剂粗制成粉,用索氏仪分别用正己烷、氯仿、甲醇等极性逐渐增大的溶剂提取。采用甲醇叶提取物对其化学成分进行分离鉴定。采用柱层析(CC)和薄层析(TLC)对化学成分进行分离纯化,并利用UV-VIS、IR、1H和13C NMR对分离得到的纯化合物进行鉴定。采用气相色谱-质谱分析鉴定其化学成分。结果分离鉴定出了大黄素、大黄酚和物理三种蒽醌类化合物。GC-MS分析鉴定了1,2-苯二羧酸二异辛基酯、甲酯、(Z, Z, Z)-9,12,15-十八碳三烯酸、硝酸壬基酯、4- c -甲基肌醇、正十六烷酸、2-甲基丁酸和十八烷酸。结论该植物中含有具有药用价值的天然活性化合物,对开发抗多种疾病的药物具有重要意义。
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引用次数: 7
A Novel Stability-Indicating Method for the Simultaneous Estimation of Saxagliptin and Dapagliflozin in Rat Serum by Using UV Spectroscopy 紫外光谱法同时测定大鼠血清中沙格列汀和达格列净含量的稳定性指示方法
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000579
Raveendra Bg, KumarRA, Shaheen Sd, A. Greeshma, M. Satyanarayana, Manikanta Rsht, Syam Cpb
A new approach developed for stability-indicating, simultaneous estimation of Saxagliptin and Dapagliflozin in rat serum by using UV spectroscopy. Saxagliptin detection wave length was at 222 nm with water is solvent and Dapagliflozin detection wave length was at 274 nm with phosphate buffer pH 6.8 is solvent. Both drugs are obeyed the beers-lamberts concentration range was founds to be 1-10 μg/mL. The present method was optimized and validated in spiked rat serum according to ICH guidelines. All validation parameters were found to be within the acceptable limits and stability-indicating studies were conducted under different conditions founds in negligible. The present method was simple and sensitive; it was successfully adopted for the simultaneous estimation of Saxagliptin and Dapagliflozin in rat serum samples by using UV spectroscopy.
建立了用紫外光谱法同时测定大鼠血清中沙格列汀和达格列净的稳定性的新方法。沙格列汀检测波长为222 nm,以水为溶剂;达格列净检测波长为274 nm,以磷酸盐缓冲液pH 6.8为溶剂。两种药物的浓度范围为1 ~ 10 μg/mL。根据ICH指南对该方法进行了优化,并在加标大鼠血清中进行了验证。所有验证参数均在可接受范围内,在不同条件下进行的稳定性研究发现可忽略不计。该方法简便、灵敏;成功地应用紫外光谱法同时测定大鼠血清样品中沙格列汀和达格列净的含量。
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引用次数: 9
Development and Validation of a HPLC Method for MS-153 Quantification: Assessment of its Stability in Rat Plasma and Brain Homogenate HPLC法测定MS-153在大鼠血浆和脑匀浆中的稳定性
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000588
Y. Wei, Bachu Rd, Y. Sari, Boddu Shs
MS-153 is a novel pyrazoline compound that serves as a potential neuroprotective therapeutic agent during ischemia. Development of a convenient, quick, and robust analytical method to quantify MS-153 in biological samples is necessary to understand it’s in vivo pharmacokinetic/pharmacodynamics (PKPD) profiles. An isocratic reverse-phase HPLC method was developed and validated for quantification of MS-153. Chromatographic separation was achieved with a C18 column. Mobile phase consisting of water/acetonitrile (85/15, v/v) was pumped at a flow rate of 1.0 mL/min. The retention time of MS-153 (λmax=260 nm) was found to be 7.15 minutes. A calibration curve established over a range of 0.78125 ng to 500 ng showed a correlation coefficient of 1.0. The LOD and LOQ were found to be 0.164 and 0.496 ng, respectively. The accuracy, intra-day precision, and inter-day precision were found to be 99.97% to 101.66% (recovery), 0.21% to 0.55% (RSD), and 0.32% to 0.82% (RSD), respectively. MS-153 was analysed from biological samples by adding methanol to remove proteins in the biological matrix prior to HPLC analysis. The extraction efficiency was found to be 100%. The developed method was also used to analyse the stability of MS-153 in diluted blank rat plasma and brain homogenate samples. Results indicated that no significant degradation of MS-153 was observed at 37°C for 6 h.
MS-153是一种新型的吡唑啉化合物,在缺血期间可作为一种潜在的神经保护治疗剂。为了了解MS-153在体内的药代动力学/药效学(PKPD)特征,有必要开发一种方便、快速、可靠的分析方法来定量生物样品中的MS-153。建立了等容反相高效液相色谱法测定MS-153的方法。采用C18色谱柱进行色谱分离。流动相为水/乙腈(85/15,v/v),以1.0 mL/min的流速泵送。MS-153 (λmax=260 nm)的停留时间为7.15 min。在0.78125 ~ 500 ng范围内建立的校准曲线的相关系数为1.0。LOD和LOQ分别为0.164和0.496 ng。准确度为99.97% ~ 101.66%(回收率),日内精密度为0.21% ~ 0.55% (RSD),日内精密度为0.32% ~ 0.82% (RSD)。MS-153是通过在HPLC分析前加入甲醇去除生物基质中的蛋白质来分析生物样品的。结果表明,提取效率为100%。该方法还用于分析MS-153在稀释的空白大鼠血浆和脑匀浆样品中的稳定性。结果表明,MS-153在37℃下发酵6 h未见明显降解。
{"title":"Development and Validation of a HPLC Method for MS-153 Quantification: Assessment of its Stability in Rat Plasma and Brain Homogenate","authors":"Y. Wei, Bachu Rd, Y. Sari, Boddu Shs","doi":"10.4172/2153-2435.1000588","DOIUrl":"https://doi.org/10.4172/2153-2435.1000588","url":null,"abstract":"MS-153 is a novel pyrazoline compound that serves as a potential neuroprotective therapeutic agent during ischemia. Development of a convenient, quick, and robust analytical method to quantify MS-153 in biological samples is necessary to understand it’s in vivo pharmacokinetic/pharmacodynamics (PKPD) profiles. An isocratic reverse-phase HPLC method was developed and validated for quantification of MS-153. Chromatographic separation was achieved with a C18 column. Mobile phase consisting of water/acetonitrile (85/15, v/v) was pumped at a flow rate of 1.0 mL/min. The retention time of MS-153 (λmax=260 nm) was found to be 7.15 minutes. A calibration curve established over a range of 0.78125 ng to 500 ng showed a correlation coefficient of 1.0. The LOD and LOQ were found to be 0.164 and 0.496 ng, respectively. The accuracy, intra-day precision, and inter-day precision were found to be 99.97% to 101.66% (recovery), 0.21% to 0.55% (RSD), and 0.32% to 0.82% (RSD), respectively. MS-153 was analysed from biological samples by adding methanol to remove proteins in the biological matrix prior to HPLC analysis. The extraction efficiency was found to be 100%. The developed method was also used to analyse the stability of MS-153 in diluted blank rat plasma and brain homogenate samples. Results indicated that no significant degradation of MS-153 was observed at 37°C for 6 h.","PeriodicalId":19833,"journal":{"name":"Pharmaceutica Analytica Acta","volume":"16 1","pages":"1-6"},"PeriodicalIF":0.0,"publicationDate":"2018-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82128999","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Understanding the importance of diversity of particle size methods based on laser diffraction 了解基于激光衍射的粒度方法多样性的重要性
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435-C4-041
pLisa Elvirip
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引用次数: 0
Role of Piperine as an Effective Bioenhancer in Drug Absorption 胡椒碱作为有效的生物促进剂在药物吸收中的作用
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000591
Mhaske Db, Sreedharan S, Mahadik Kr
Bioenhancers can be defined as chemical entities, which when mixed with drugs promote and augment their bioavailability without showing any synergistic effect with the drug. The factors like toxicity, cost, poor bioavailability and long term administration of drugs give rise to the need of bioenhancers which help overcome most of these problems. Piper species produce a pungent alkaloid named Piperine or 1-peperoyl piperidine. Piperine increases permeability at the site of absorption by modulating lipid environment and membrane dynamics. Piperine has a molecular structure that is suitable for enzyme inhibition. It augments the bioavailability of several drugs like carbamazepine, curcumin, ciprofloxacin, ampicillin, metronidazole, oxytetracycline and many others by inhibiting various metabolizing enzymes. Thus piperine, being an efficacious inhibitor of drug metabolism is a powerful enhancer of absorption. The following review explores the mechanism, metabolism inhibition, influence of structural changes on activity, and drugs bioenhanced by piperine. It provides an insight on the application of piperine as an effective bioenhancer and the superiority of a bioenhanced drug formulation over the one without a bioenhancer. This concept which is found to be beneficial, has its roots in Ayurveda-the traditional Indian system of medicine and has been applied to various drugs. It presents a fine instance of the advantage of amalgamating a traditional system with contemporary medicine.
生物增强剂可以定义为化学实体,当与药物混合时,它可以促进和增加药物的生物利用度,而不会与药物产生任何协同效应。药物的毒性、成本、生物利用度差和长期给药等因素导致对生物增强剂的需求,这有助于克服大多数这些问题。胡椒种产生一种刺激性的生物碱,称为胡椒碱或1-胡椒酰胡椒碱。胡椒碱通过调节脂质环境和膜动力学来增加吸收部位的渗透性。胡椒碱具有适合酶抑制的分子结构。它通过抑制各种代谢酶来提高卡马西平、姜黄素、环丙沙星、氨苄西林、甲硝唑、土霉素和许多其他药物的生物利用度。因此,胡椒碱作为一种有效的药物代谢抑制剂,是一种强大的吸收促进剂。下面就胡椒碱的作用机制、代谢抑制、结构变化对活性的影响以及胡椒碱的生物增强药物进行综述。它提供了胡椒碱作为一种有效的生物增强剂的应用和生物增强药物配方优于不含生物增强剂的药物配方的见解。人们发现,这种有益的概念源于印度传统医学体系阿育吠陀,并已应用于各种药物。这是传统医学与现代医学相结合的一个很好的例子。
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引用次数: 30
Development and Evaluation of Dual Release Tablet of Metformin and Pioglitazone for the Treatment of Diabetes Mellitus 二甲双胍吡格列酮双缓释片治疗糖尿病的研制与评价
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000583
Mhase, B. Nanjwade, Arindam Sarkar, T. Srichana
The objective of present work is to develop and characterize dual release tablet formulation containing Metformin in extended release matrix form and Pioglitazone in immediate release form for the treatment of Diabetes mellitus. Different formulations containing Metformin HCl were manufactured using 32 factorial designs. Influences of hydrophobic carrier, hydrophilic polymer on drug release were studied. Immediate release layer of Pioglitazone was optimized using different disintegrants. All formulations were evaluated for percentage drug release and analyzed according to various release kinetic models. Optimization results indicated that release rate of Metformin is directly proportional to the levels of stearic acid (SA) and poly-ethylene-oxide (PEO). Kinetic analysis showed that formulation M6 was good releasing with f2 value of 81.08 and follows Higuchi and Peppas model with correlation coefficient value 0.9780 and 0.9910 respectively. Similarly, optimization study indicated that release of Pioglitazone is dependent on the level and type of disintegrant, formulation P5 shown highest f2 value of 84.08. Results confirmed that dual-release inlay-tablet formulation containing extended release of Metformin HCl and immediate release of Pioglitazone HCl could be developed for the treatment of Diabetes mellitus.
本研究的目的是研制治疗糖尿病的二甲双胍缓释基质和吡格列酮速释双释放片剂。采用32因子设计制备含盐酸二甲双胍的不同配方。研究了疏水载体、亲水性聚合物对药物释放的影响。采用不同的崩解剂对吡格列酮的速释层进行优化。评价各制剂的释药百分率,并根据各种释药动力学模型进行分析。优化结果表明,二甲双胍的释放率与硬脂酸(SA)和聚环氧乙烷(PEO)的含量成正比。动力学分析表明,配方M6释放效果良好,f2值为81.08,符合Higuchi和Peppas模型,相关系数分别为0.9780和0.9910。同样,优化研究表明,吡格列酮的释放度与崩解剂的含量和类型有关,配方P5的f2值最高,为84.08。结果证实,具有盐酸二甲双胍缓释和盐酸吡格列酮速释双重缓释嵌片制剂可用于糖尿病的治疗。
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引用次数: 2
Bacterial Electrode for the Oxidation and Detection of Phenol 细菌电极对苯酚的氧化和检测
Pub Date : 2018-01-01 DOI: 10.4172/2153-2435.1000580
R. Maallah, A. Chtaini
Voltametric degradation of phenol was carried out at microbial electrode. This electrode is based on graphite carbon and natural phosphate modified by bacteria inserted in the phosphate matrix, the whole is covered by a polymer developed in situ on the surface. This electrode, designated subsequently by bacteria-NP-CPE, Showed stable response and was characterized with voltametric methods, as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The experimental results revealed that the prepared electrode could be a feasible for degradation of hazardous phenol pollutants.
在微生物电极上进行了苯酚的伏安降解。该电极是以石墨碳和天然磷酸盐为基础,经细菌修饰后插入磷酸盐基质中,整体表面覆盖一层原位发育的聚合物。该电极经细菌- np - cpe鉴定,反应稳定,并用循环伏安法(CV)和电化学阻抗谱(EIS)等伏安方法进行了表征。实验结果表明,所制备的电极对有害酚类污染物的降解是可行的。
{"title":"Bacterial Electrode for the Oxidation and Detection of Phenol","authors":"R. Maallah, A. Chtaini","doi":"10.4172/2153-2435.1000580","DOIUrl":"https://doi.org/10.4172/2153-2435.1000580","url":null,"abstract":"Voltametric degradation of phenol was carried out at microbial electrode. This electrode is based on graphite carbon and natural phosphate modified by bacteria inserted in the phosphate matrix, the whole is covered by a polymer developed in situ on the surface. This electrode, designated subsequently by bacteria-NP-CPE, Showed stable response and was characterized with voltametric methods, as cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The experimental results revealed that the prepared electrode could be a feasible for degradation of hazardous phenol pollutants.","PeriodicalId":19833,"journal":{"name":"Pharmaceutica Analytica Acta","volume":"480-481 1","pages":"1-6"},"PeriodicalIF":0.0,"publicationDate":"2018-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77853067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 10
期刊
Pharmaceutica Analytica Acta
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