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Validated RP-HPLC-PDA method for simultaneous determination of Zidovudine, Lamivudine, and Nevirapine in pharmaceutical formulation 验证了RP-HPLC-PDA同时测定制剂中齐多夫定、拉米夫定和奈韦拉平含量的方法
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148890
B. Ishaq, K. Prakash, G. Mohan
Aim and Objectives: A simple, rapid, and sensitive high performance liquid chromatographic method with ultraviolet detection has been developed and validated according to the International Conference on Harmonization (ICH) guidelines for the quantitation and qualification of zidovudine (ZID), lamivudine (LAM), and nevirapine (NEV) in pharmaceutical dosage forms. Materials and Methods: The proposed method was based on the separation of the drugs in reversed phase mode using Water′s C18 250 cm × 4.6 mm, 5 μ particle size column maintained at an ambient temperature. The optimum mobile phase consisted of Water: Methanol (70:30 v/v), pH adjusted to four with orthophosphoric acid (OPA). The flow rate of mobile phase was set 1.0 mL min -1 and photodiode array detection was performed at 275 nm with a total run time of 8 min which is very short for accurate analysis of simultaneous estimation of three analytes. The method was validated according to ICH guidelines. Results: The method was linear over the concentration range of 25-75 μg mL -1 with limit of quantifications (LOQ) of 13, 0.49, and 0.40 ng mL -1 for ZID, LAM and NEV respectively and limit of detection (LOD) of 4, 0.14, and 0.12 ng mL -1 for ZID, LAM and NEV respectively. Accuracy (% recovery studies) and precision values of both inter and intraday obtained from six different replicates for all the analytes ranged from 99.00% to 100.00% and % relative standard deviation of precision (assay) was between 0.64 and 1.28, respectively. All the three analytes and their combination drug product were exposed to thermal, photolytic, hydrolytic, reductive, oxidative and peroxide stress conditions and the stressed samples were analyzed by the proposed method. There were no interfering peaks from excipients, impurities or degradation products due to variable stress conditions and the proposed method is specific for the simultaneous estimation of ZID, LAM and NEV in the presence of their degradation products. Conclusion: The proposed method can be successfully applied in the quality control and stability samples of pharmaceutical dosage forms.
目的:根据国际统一会议(ICH)药品剂型中齐多夫定(ZID)、拉米夫定(LAM)和奈韦拉平(NEV)的定量鉴定指南,建立了一种简单、快速、灵敏的紫外检测高效液相色谱方法,并进行了验证。材料与方法:采用Water公司的C18 250 cm × 4.6 mm,粒径5 μ的色谱柱,在常温下进行反相分离。最佳流动相为水:甲醇(70:30 v/v),以正磷酸(OPA)调节pH为4。流动相流速为1.0 mL min -1,在275 nm处进行光电二极管阵列检测,总运行时间为8 min,对于同时估计三种分析物的准确分析非常短。根据ICH指南对方法进行了验证。结果:该方法在25 ~ 75 μg mL -1的浓度范围内呈线性关系,ZID、LAM和NEV的定量限分别为13、0.49、0.40 ng mL -1, ZID、LAM和NEV的检出限分别为4、0.14、0.12 ng mL -1。所有分析物6个不同重复的准确度(回收率研究)和精密度值在99.00% ~ 100.00%之间,精密度(测定)的相对标准偏差在0.64 ~ 1.28之间。在热、光解、水解、还原、氧化和过氧化等应激条件下,对三种分析物及其联合产物进行分析。由于不同的应力条件,没有来自辅料、杂质或降解产物的干扰峰,该方法适用于同时估计ZID、LAM和NEV存在降解产物的情况。结论:该方法可成功地应用于药品剂型的质量控制和稳定性检验。
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引用次数: 3
Formulation variable study and optimization of taste masked mouth dissolving tablets using design of experiment 用实验设计法对味掩口溶片的配方变量进行研究与优化
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148887
V. Sharma, L. Singh
Background: Aim of present work is to prepare and optimized mouth dissolving tablets (MDTs) by using tasteless complex of levocetirizine. Materials and Methods: Formulation and optimization of tablets was done by using computer optimization technique. Formulated taste masked complex of drug was characterized by taste evaluation, percentage drug loading, thermal analysis and X-ray diffraction pattern. Optimization of MDTs was done by considering concentration of binder (polyvinylpyrrolidone [PVP] K30) and super-disintegrant (Kyron T-314) as independent variables whereas wetting time (WT), friability (Fr) and amount of drug release in 15 m (Q 15 ) as dependent variables. Response surface plots and contour plots were drawn, and optimum formulations were selected by feasibility and grid searches. Result and Discussion: By using 3 2 central composite design (CCD) optimized batch was obtained for which value of independent variable, PVP K30 (X1) and Kyron T-314 (X2) was 15 mg and 21 mg respectively and for dependent response, that is, Fr, WT and Q 15 to be 0.42%, 11.8 s. and 91.16% respectively. Validation of optimization study indicated very high degree of prognostic ability of response surface methodology (RSM). By analyzing the observed value to predicted value for Fr, WT and Q 15 the regression coefficient value was found to be 0.950, 0.961 and 0.957. Linearity of plot concluded that desired predicted response of all check-point batches were close to the predicted values and show the validity of data. Conclusion: Hence, optimized formulated batches were formulated by proper balancing of concentration of independent variables to attain desired dependent response using 3 2 CCD. Thus, 3 2 CCDs is an efficient tool in optimization experiments. High degree of outcome obtained using RSM concludes that 3 2 CCD is quite efficient in optimizing drug delivery systems that exhibit nonlinearity in response.
背景:利用无味的左西替利嗪复配物制备口腔溶出片并对其进行优化。材料与方法:采用计算机优化技术对片剂的处方进行优化。通过口感评价、载药量百分比、热分析和x射线衍射等方法对配制的掩味复合物进行表征。以黏结剂(聚乙烯吡咯烷酮[PVP] K30)浓度和超崩解剂(Kyron T-314)浓度为自变量,以润湿时间(WT)、脆性(Fr)和15 m内药物释放量(Q 15)为因变量,对MDTs进行优化。绘制响应面图和等高线图,通过可行性搜索和网格搜索选择最优配方。结果与讨论:采用32个中心复合设计(CCD),获得了自变量PVP K30 (X1)和Kyron T-314 (X2)分别为15 mg和21 mg,依赖响应为Fr、WT和q15分别为0.42%、11.8 s和91.16%的优化批次。优化研究的验证表明响应面法(RSM)具有很高的预测能力。通过对Fr、WT和q15的观测值与预测值进行分析,回归系数分别为0.950、0.961和0.957。图的线性关系表明,各检查点批次的期望预测响应接近预测值,表明数据的有效性。结论:通过合理平衡各自变量的浓度,通过32 - 2 CCD获得所需的依赖响应,可优选出最佳制剂批次。因此,3.2 ccd是优化实验的有效工具。使用RSM获得的高程度结果表明,32 CCD在优化具有非线性响应的给药系统方面非常有效。
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引用次数: 2
Antibacterial potency of Ziziphus mauritiana (Fam-Rhamnaceae) roots 毛里沙普根的抑菌作用
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148895
S. Upadhyay, A. Mishra, Srishti Srivastava, P. Upadhyay, A. Ghosh, Vijender Singh
Background: Ziziphus mauritiana is a well known herb generally its fruit is used in stomach ailments or infections.The genus Ziziphus is known for its antimicrobial potency. Material and Methods: Here Z. mauritiana roots were taken for conducting experiments in various bacterial strains for evaluating its antibacterial potency by disc diffusion method. The minimum inhibitory concentration and zone of inhibition were also determined. The mode of action was determined by leakage of nucleic acid and its determination by UV spectrometry. Results: The root extract of Z.mauritiana posses excellent antibacterial activity against as the activity is well compared with standard drug ciprofloxacin. The mode of action of the extract was bactericidal. Conclusion: Effective and safe herbal antibiotic may be produced in the future by root extract of Z.mauritiana.
背景:毛里求斯酸枣是一种众所周知的草药,其果实通常用于胃病或感染。Ziziphus属以其抗菌效力而闻名。材料与方法:本实验采用圆盘扩散法,取毛竹根在不同菌株中进行抑菌效果实验。确定了最低抑菌浓度和抑菌区。采用核酸泄漏法和紫外光谱法测定其作用方式。结果:牡丹根提取物具有良好的抑菌活性,其抑菌活性优于标准药物环丙沙星。提取物的作用方式是杀菌。结论:毛里塔纳根提取物可用于生产安全有效的中药抗生素。
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引用次数: 0
Stability indicating high performance thin layer chromatographic method for quantitation of venlafaxine in bulk and pharmaceutical dosage form 稳定性表明高效薄层色谱法定量散装和药物剂型文拉法辛
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148891
S. Dubey, A. Anand, R. Saha
Background: Venlafaxine (VEN) is a phenethylamine bicyclic compound, chemically, 1-(2-[dimethyl amino]-1-[4-methoxy phenyl] ethyl) cyclo-hexan-1ol hydrochloride. It is a antidepressant. It inhibits the reuptake of serotonin, nor adrenaline and dopamine to a lesser extent at the presynaptic membrane. Aim: A simple, rapid, precise, accurate, and economical high performance thin layer chromatographic (HPTLC) method has been developed and validated for the determination of VEN both as a bulk drug and in formulation. Materials and Methods: The method uses aluminum plates precoated with silica gel 60 F254 as the stationary phase and dichloromethane:acetonitrile:N-hexane:triethylamine: 0.5:0.5:4:0.7 (v/v/v/v) as mobile phase. Results: This system gave compact spots for VEN (R f = 0.46 ± 0.05). Forced degradation studies were done by subjecting VEN to acid and alkali hydrolysis, oxidation, and reduction. The peak of the degradation product was well resolved from that of the pure drug and had significant different R f values. Analysis of VEN was performed in the absorbance mode at 225 nm. The limit of detection and quantification were 12.48 and 37.81 ng/spot respectively. Conclusions: The developed method was validated and found to be simple, specific, accurate and precise and can be used for routine quality control analysis of VEN in bulk and pharmaceutical formulation.
背景:文拉法辛(Venlafaxine, VEN)是一种苯乙胺双环化合物,化学性质为1-(2-[二甲基氨基]-1-[4-甲氧基苯基]乙基)环己醇盐酸盐。它是一种抗抑郁药。它抑制5 -羟色胺的再摄取,也抑制肾上腺素和多巴胺在突触前膜的再摄取。目的:建立一种简便、快速、精确、准确、经济的高效薄层色谱(HPTLC)方法,用于原料药和制剂中VEN的测定。材料与方法:该方法以预涂硅胶60f254的铝板为固定相,二氯甲烷:乙腈:正己烷:三乙胺:0.5:0.5:4:7 0 (v/v/v/v)为流动相。结果:该系统的VEN斑点排列紧凑(R f = 0.46±0.05)。强迫降解研究是通过使VEN经受酸碱水解、氧化和还原来完成的。降解产物的峰与纯药物的峰分离较好,且R f值差异显著。在225 nm吸光度模式下对VEN进行分析。检测限为12.48 ng/点,定量限为37.81 ng/点。结论:所建立的方法简便、专属性强、准确度高,可用于VEN原料药和制剂的常规质量控制分析。
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引用次数: 2
Total protein in gingival crevicular fluid as indicators of periodontal disease activity: A clinico biochemical analysis 龈沟液中总蛋白作为牙周病活动性指标的临床生化分析
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148885
A. Koregol, Shobha More, Savita Koregol, Nagaraj B Kalburgi
Background: Gingival crevicular fluid (GCF) is regarded as a promising medium for detection of markers of periodontal disease activity. Very few investigators have examined concentration of total protein in GCF, but most results are not in agreement to one another. Aim: This study was undertaken to quantitatively estimate total protein concentration of GCF in gingivitis and periodontitis and to find reliability of these as diagnostic markers of disease activity. This will indicate the stage of disease activity, help in early diagnosis, prevention and treatment of periodontal diseases. Materials and Methods: Study included patients between 18 and 55 years, divided into two groups: Gingivitis (Group-I) and periodontitis (Group-II). Using volumetric micro capillary pipette 1 μl GCF was collected for quantitative analysis of total protein using spectrophotometry. Results: The concentration of total protein in GCF and their significant correlation with gingival index, pocket depth measurements, reflects the clinical status of gingival and periodontal tissues. Conclusions: Estimation of proteins may be used as potential diagnostic markers of active disease status in periodontal tissues and to predict effective methods of prevention and treatment.
背景:龈沟液(GCF)被认为是一种很有前途的检测牙周病活动标志物的介质。很少有研究者检测过GCF中总蛋白的浓度,但大多数结果并不一致。目的:本研究旨在定量估计牙龈炎和牙周炎中GCF的总蛋白浓度,并发现这些作为疾病活动性诊断指标的可靠性。这将表明疾病活动的阶段,有助于早期诊断、预防和治疗牙周病。材料与方法:研究对象为18 ~ 55岁的患者,分为牙龈炎组(i组)和牙周炎组(ii组)。取1 μl GCF,用分光光度法对总蛋白进行定量分析。结果:GCF中总蛋白浓度与牙龈指数、袋深测量值有显著相关性,反映了牙龈及牙周组织的临床状况。结论:蛋白质的测定可作为牙周组织活动性疾病状态的潜在诊断指标,并预测有效的预防和治疗方法。
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引用次数: 6
Phytochemical evaluation of the ethanolic extracts of some Nigerian herbal plants 尼日利亚几种草本植物乙醇提取物的植物化学评价
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148882
E. Chinedu, Arome David, S. Ameh
Background: Herbs basically, are plants or plant parts employed due to their scent, medicinal properties or flavor. Herbal medicines have longed been used in the management and treatment of various ailments even before the arrival of modern medicine. Herbal medicines are still being used today, as it has even gained a new momentum in the field of medicine. Phytochemicals are responsible for eliciting definite physiological effects of various herbs in the body. In Nigeria, various plants are being used traditionally in the treatment of divers ailments. Some of these plants include Tapinanthus bangwensis, Tamarindus indica, Ocimum gratissimum, Allium sativum, Kigelia africana, Azadirachta indica, Solanum virginianum, Myrianthus serratus and Vernonia amygdalina. Though there have been claims of success in their traditional usage, it is however important to carry-out phytochemical assessment on them. Aim: The aim was to evaluate the phytochemical constituents of the ethanolic extract of these plants. Materials and Methods: The plant materials were extracted, and the plant extracts were screened for the presence of various phytochemical constituents such as alkaloids, steroids, glycosides, cardiac glycosides, flavonoids, carbohydrate, saponins, tannins and anthraquinones using the standard methods. Result: The experimental result revealed the presence of the various bioactive phytochemicals in the different plant extracts investigated. These phytochemicals were however present in different proportions in the various plant extracts. Conclusion: The experimental result vindicates the usage of these plants traditionally for medicinal purposes.
背景:草药基本上是植物或植物部分,由于它们的气味,药用特性或风味而被使用。早在现代医学出现之前,草药就一直被用于治疗各种疾病。草药今天仍在使用,因为它甚至在医学领域获得了新的动力。植物化学物质负责引发体内各种草药的明确生理作用。在尼日利亚,传统上使用各种植物来治疗各种疾病。其中一些植物包括:班文山芋、柽柳、山竹、葱、非洲木、印楝、维吉尼亚茄、千里马和扁桃。虽然传统的使用方法取得了成功,但对它们进行植物化学评估是很重要的。目的:评价这些植物乙醇提取物的化学成分。材料与方法:提取植物材料,采用标准方法筛选植物提取物中生物碱、甾体、糖苷、心苷、黄酮类化合物、碳水化合物、皂苷、单宁、蒽醌类等多种植物化学成分。结果:实验结果揭示了所研究的不同植物提取物中存在多种具有生物活性的植物化学物质。然而,这些植物化学物质以不同比例存在于各种植物提取物中。结论:实验结果证明了这些植物的传统药用价值。
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引用次数: 9
Histopathological alterations in the vital organs of Indian Major Carps with parasitic infestation in fish farms West Bengal, India 印度西孟加拉邦养鱼场寄生虫感染的印度主要鲤鱼重要器官的组织病理学改变
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148893
K. Ramudu, G. Dash
The study was conducted to investigate the histological changes of vital organs such as kidney, gills and brain with the mixed infestation of parasites in Indian Major Carps (IMC). The parasites such as Myxobolus spp., Thelohanellus spp., Trichodina spp., Dactylogyrus spp., Gyrodactylus spp. and Nematodes were observed in three IMC. Several histological alterations were observed in the kidney of Catla catla, Labeo rohita and Cirrhinus mrigala, which includes vacuolar degeneration in the epithelium of renal tubules, focal areas of necrosis, proliferation of bowman′s capsule and many cases the renal tubules lost its shape and canalculi formation was observed. The gills showed focal areas of necrosis, exacerbated swelling of gill arch, deposition of distinct black melanin pigmentation at the basal point of the gill arch, loss of primary and secondary lamellae, prominent vacuolar degeneration and formation of vacuoles. The presence of protozoan parasites in brain tissue resulted necrosis of the brain tissue, black pigmentation, vacuolization of myelin sheath of nerve fibers and common degenerative changes. Aims: To study histological changes of vital organs such as kidney, gills and brain with the mixed infestation of parasites in Indian Major Carps (IMC). Settings and Design: The organs fixed in 4% formalin are transferred to 50% ethyl alcohol and stored for further analysis. Materials and Methods: Histopathological analysis was made as described by Roberts. Statistical Analysis Used: Nil. Results: Described in text. Conclusions: The present study brings about conclusion that impact of mixed infestation of the parasites on their hosts was severe. Histopathological changes were observed in vital organs which might be due to toxins released by different parasites or physical damage of tissue with the presence of parasites.
研究了寄生虫混合侵染后印度大鲤鱼(IMC)肾脏、鳃和脑等重要器官的组织学变化。在3个IMC中均观察到黏液菌属、带菌菌属、毛霉属、长趾菌属、旋毛虫属和线虫等寄生虫。猫、鼠、麻鼠肾脏组织学改变主要表现为肾小管上皮空泡变性、局灶性坏死、鲍曼囊增生,多见肾小管失形、小管形成。鳃表现为局灶性坏死,鳃弓肿胀加重,鳃弓基部有明显的黑色黑色素沉积,初级和次级片片缺失,明显的空泡变性和液泡形成。脑组织中存在原生动物寄生虫,导致脑组织坏死、黑色色素沉着、神经纤维髓鞘空泡化和常见的退行性改变。目的:研究寄生虫混合侵染印度大鲤鱼(IMC)后肾、鳃、脑等重要器官的组织学变化。设置和设计:将在4%福尔马林中固定的器官转移到50%乙醇中保存以供进一步分析。材料和方法:按照Roberts的描述进行组织病理学分析。统计分析用途:无。结果:文字描述。结论:寄生虫混合侵染对寄主的影响是严重的。在重要器官中观察到组织病理学变化,这可能是由于不同寄生虫释放的毒素或寄生虫存在对组织的物理损伤。
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引用次数: 4
Formulation and evaluation of sustained release matrix tablets of pioglitazone hydrochloride using processed Aloe vera mucilage as release modifier 以芦荟胶浆为缓释剂的盐酸吡格列酮缓释基质片的研制与评价
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148881
M. Choudhary, T. Salukhe, A. Ganeshpurkar, V. Pandey, Nazneen Dubey, D. Bansal
Background: Natural gums and mucilage which hydrates and swells on contact with aqueous media are used as additives in the formulation of hydrophilic drug delivery system. Aim: The purpose of this study was to develop a new monolithic matrix system for complete delivery of Pioglitazone hydrochloride (HCl), in a zero-order manner over an extended time period using processed Aloe vera gel mucilage (PAG) as a release modifier. Materials and Methods: The matrices were prepared by dry blending of selected ratios of polymer and ingredients using direct compression technique. Physicochemical properties of dried powdered mucilage of A. vera were studied. Various formulations of pioglitazone HCl and A. vera mucilage were prepared using different drug: Polymer ratios viz., 1:1, 1:2, 1:3, 1:4, 1:5 for PAG by direct compression technique. Results: The formulated matrix tablets were found to have better uniformity of weight and drug content with low statistical deviation. The swelling behavior and in vitro release rate characteristics were also studied. Conclusion: The study proved that the dried A. vera mucilage can be used as a matrix forming material for controlled release of Pioglitazone HCl matrix tablets.
背景:天然树胶和黏液在与水介质接触时会发生水化和膨胀,它们被用作亲水性给药系统配方的添加剂。目的:本研究的目的是开发一种新的单片基质系统,用于在长时间内以零级方式完全释放盐酸吡格列酮(HCl),使用加工过的芦荟凝胶粘液(PAG)作为释放调节剂。材料与方法:采用直接压缩技术,将选定比例的聚合物与原料干共混制备基质。研究了芦荟干粉末状粘液的理化性质。采用直接压缩技术制备了盐酸吡格列酮和真丝草胶的不同药物聚合物比,即PAG的1:1、1:2、1:3、1:4、1:5。结果:所制基质片重量均匀性好,含量均匀性好,统计偏差小。并对其溶胀行为和体外释放率特性进行了研究。结论:研究证明,干燥的真丝草粘液可作为盐酸吡格列酮基质片控释的基质形成材料。
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引用次数: 2
Spectrophotometric method for simultaneous estimation of atazanavir sulfate and ritonavir in tablet dosage form 分光光度法同时测定片剂中硫酸阿扎那韦和利托那韦的含量
Pub Date : 2015-01-01 DOI: 10.4103/2394-2002.148880
Disha A. Patel, B. Patel, C. Patel
Background: Ritonavir (RTV) and atazanavir sulfate (ATV) are protease inhibitor and RTV mostly used as a booster for increasing the bioavailability of other protease inhibitors like ATV. Aims: Quality assessment of the new dosage form of RTV and ATV i.e., tablets is very essential and hence this work deals with to develop sensitive, simple and precise method for simultaneous estimation of ATV and RTV in tablet dosage form by absorbance correction method. Materials and Methods: The present work was carried out on Shimadzu Ultraviolate(UV)-1700 double beam spectrophotometer with 1 cm path length supported by S Shimadzu, model-1700(Japan), UV-Probe software, version 2.31 was used for spectral measurements with 10 mm matched quartz cells. Standard ATV and RTV were supplied by Cipla Pharmaceutical Ltd. Methanol was purchased from Finar Chemicals Pvt. Ltd. Results and Conclusion: The λmax or the absorption maxima for ATV and RTV were found to be 279 and 240 nm, respectively in methanol as solvent. The drugs follow Beer-Lambert′s law in the concentration range 30-90 and 10-30 μg/mL for ATV and RTV, respectively. The percentage recovery was found to be 100-100.33% and 100-101.5% for ATV and RTV, respectively. The method was validated for different parameters as per the International Conference for Harmonization Guidelines.
背景:利托那韦(RTV)和硫酸阿扎那韦(ATV)是蛋白酶抑制剂,RTV主要用作提高其他蛋白酶抑制剂如ATV的生物利用度的助推器。目的:对新剂型即片剂进行质量评价是十分必要的,因此本工作旨在建立一种灵敏、简便、精确的吸光度校正法同时测定片剂剂型中亚硝胺和亚硝胺含量的方法。材料与方法:采用日本Shimadzu紫外-1700双光束分光光度计,光路长度为1 cm,型号为S Shimadzu -1700,采用2.31版UV- probe软件对10 mm匹配的石英细胞进行光谱测量。标准ATV和RTV由Cipla制药有限公司提供。甲醇购自Finar Chemicals Pvt. Ltd.。结果与结论:以甲醇为溶剂,ATV和RTV的λmax分别为279 nm和240 nm。ATV和RTV的浓度范围分别为30 ~ 90 μg/mL和10 ~ 30 μg/mL,符合Beer-Lambert定律。ATV和RTV的回收率分别为100 ~ 100.33%和100 ~ 101.5%。根据国际协调准则会议,对该方法进行了不同参数的验证。
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引用次数: 6
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Drug Development and Therapeutics
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