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Two Dimensional Gas Chromatography- A Review 二维气相色谱-综述
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00050
K. B. Sri, G. Shailaja, M. Sumakanth
The birth of two-dimensional gas chromatography is assumed to be the ninetieth year of the last century. Two-dimensional gas chromatography is a rapidly developing analytical technique. GCxGC is a truly hyphenated chromatographic technique which employs a pair of GC column. GCxGC analyses, such as the identification of trace compounds that would not be perceived by 1D-GC. The use of 2D-GC compared to that of 1D-GC has been discussed. The paper presents the introduction, principle of operation, working, uses, application, case studies has been discussed.
二维气相色谱法的诞生被认为是在上世纪九十年代。二维气相色谱是一种发展迅速的分析技术。GCxGC是一种真正的联用色谱技术,它采用一对气相色谱柱。GCxGC分析,例如鉴定1D-GC无法检测到的微量化合物。讨论了二维气相色谱与一维气相色谱的应用。本文介绍了该系统的介绍、工作原理、工作原理、用途、应用,并对实例进行了讨论。
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引用次数: 1
Degradation Profiling of Lisinopril and Hydrochlorothiazide by RP- HPLC method with QbD Approach QbD法反相高效液相色谱法分析赖诺普利和氢氯噻嗪的降解特性
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00046
Kalleshvar P. Jatte, R. Chakole, M. Charde
RP-HPLC method was developed for the estimation of Lisinopril and Hydrochlorothiazide in tablet dosage form with the help of Quality by Design (QbD) approaches. In this method concentration of each drug was obtained by using the absorptivity values calculated for drug wavelength 226.0 nm and solving the equation. The RP-HPLC method was performed C18-(100mm x 4.6 mm,)2.5 μm particle size in gradient mode, and the sample was analysed using methanol 45.0 ml and 55.0 ml (pH 3.3 0.05% OPA with TEA) as a mobile phase at a flow rate of 0.8 ml/min and detection at nm. By the retention time for Lisinopril and Hydrochlorothiazide found 3.39 and 4.59 min respectively. Validation related the method is specific, rapid, accurate, precise, reliable, and reproducible. Calibration plots by both HPLC were linear over the 5-25 and 12.5-62.5 μg/ml for Lisinopril and Hydrochlorothiazide respectively, and recoveries from tablet dosage form were between 99.02 and 100.00 %. The method can be used for routine of the quality control in pharmaceuticals. The degradation profiling of Lisinopril and Hydrochlorothiazide were also carried out.
建立了以质量设计法(QbD)评价赖诺普利和氢氯噻嗪片剂剂型的反相高效液相色谱法。该方法在药物波长226.0 nm处计算各药物的吸光度值,通过求解方程得到各药物的浓度。反相高效液相色谱(RP-HPLC):粒径为C18-(100mm × 4.6 mm,)2.5 μm,梯度模式,以甲醇45.0 ml和55.0 ml (pH为3.3,0.05% OPA, TEA)为流动相,流速为0.8 ml/min, nm检测。赖诺普利和氢氯噻嗪的保留时间分别为3.39和4.59 min。验证相关方法具有特异性、快速、准确、精密度、可靠性和可重复性。赖诺普利和氢氯噻嗪在5 ~ 25 μg/ml和12.5 ~ 62.5 μg/ml范围内均呈线性关系,片剂加样回收率在99.02 ~ 100.00%之间。该方法可作为药品质量控制的常规方法。对赖诺普利和氢氯噻嗪进行了降解分析。
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引用次数: 0
Antimicrobial Activity of Synthesized Zinc Oxide Nanoparticles using Ajuga bracteosa Leaf Extract 小苞草叶提取物合成氧化锌纳米颗粒的抗菌活性研究
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00047
M. Purohit, Anuj Kandwal, Reena Purohit, A. R. Semwal, Parveen Shama, A. Khajuria
Nanoscience and nanotechnology has attracted a lot of attention because of its wide variety of applications. Plant based metallic nanoparticles revolutionized the health sector with targeting nano drug to cure different ailments. Living beings are known to be susceptible to microbial attack followed by multidrug resistance of microorganism put the necessitates for searching more efficient methods of drug delivery or drug production. In the present study, we report the green synthesis of stable hexagonally shaped zinc oxide nanoparticles from leaf extract of Ajuga bracteosa and their antimicrobial efficacy against the selected bacterial (Streptococcus pneumonia, Staphylococcus aureus, Klebsiella pneumonia, Escherichia coli and Pseudomonas aeruginosa) and fungal (Aspergillus fumigates and Trichoderma viride) strains by using agar well diffusion method. Initial colour change and surface-plasmon-resonance (SPR) absorbance bands between 349 nm gave support to the synthesis of zinc oxide nanoparticles. These nanoparticles were further characterized by XRD, EDX, TEM and FTIR techniques. XRD analysis showed that nanoparticles are crystalline in nature. TEM measurements showed that nanoparticles are hexagonally shaped with their average size less than 27 nm. FTIR spectra confirms the presence of phytochemicals which were responsible for reducing, capping and stabilizing the nanoparticles. Antimicrobial results of the synthesized ZnO nanoparticles has indicated the good potential of nanoparticles against all tested microorganism in the present study.
纳米科学和纳米技术由于其广泛的应用而引起了人们的广泛关注。以植物为基础的金属纳米颗粒通过靶向纳米药物治疗不同的疾病,彻底改变了卫生部门。生物容易受到微生物的攻击,随之而来的是微生物的多药耐药,这就需要寻找更有效的给药或药物生产方法。本研究采用琼脂孔扩散法,绿色合成了稳定的六角形氧化锌纳米颗粒,并对选定的细菌(肺炎链球菌、金黄色葡萄球菌、肺炎克雷伯菌、大肠杆菌和铜绿假单胞菌)和真菌(烟熏曲霉和绿色木霉)进行了抑菌效果研究。初始颜色变化和349 nm之间的表面等离子体共振(SPR)吸收带支持了氧化锌纳米颗粒的合成。采用XRD、EDX、TEM和FTIR等技术对纳米颗粒进行了进一步表征。XRD分析表明,纳米颗粒具有结晶性质。TEM测量表明,纳米颗粒呈六边形,平均尺寸小于27 nm。FTIR光谱证实了植物化学物质的存在,这些化学物质负责还原、封盖和稳定纳米颗粒。合成的氧化锌纳米颗粒的抑菌实验结果表明,该纳米颗粒具有良好的抑菌潜力。
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引用次数: 9
A Review on GC-MS Hyphenated Technique GC-MS联用技术研究进展
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00049
P. Thakur, U. Thakur, Pooja Kaushal, A. Ankalgi, Pramod Kumar, Aman Kapoor, Mahendra Singh Ashawat
The hyphenated technique is developed from the coupling of a separation technique and an on-line spectroscopic detection technology, GCMS, LC-MS, LC-FTIR, LC-NMR, and CE-MS. Gas chromatography combined with mass spectrometry is an important technique for identification and quantification of analytes in multifactor systems. GC-MS is highly effective and versatile analytical techniques with numerous scientific applications to cater the field of applied Sciences and Technology. This review elaborates the significant uses of this technique. It includes a brief discussion of the instrumental set-up and theory for the comprehensive GC × GC hyphenated with different detection techniques. It is fast and sensitive, provides a high peak capacity, and allows determination of thermally stable and volatile compounds.
联用技术是由分离技术和在线光谱检测技术(GCMS、LC-MS、LC-FTIR、LC-NMR和CE-MS)耦合发展而来的。气相色谱-质谱联用技术是多因素系统中分析物鉴别和定量的重要技术。GC-MS是一种高效、通用的分析技术,具有众多的科学应用,以满足应用科学和技术领域的需求。本文详细介绍了该技术的重要用途。简要讨论了综合气相色谱×气相色谱联用不同检测技术的仪器设置和原理。它是快速和敏感的,提供了一个高的峰值容量,并允许热稳定和挥发性化合物的测定。
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引用次数: 4
Bioanalysis - Method Development, Validation, Sample Preparation, its Detection Techniques and its Application 生物分析-方法发展,验证,样品制备,其检测技术及其应用
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00051
Seema R. Nikam, Amol S. Jagdale, S. Boraste, Shrikant B Patil
Quantitatively measurements of chemical and biological drugs and their metabolites in the biological sample. This used in clinical and non-clinical studies. Non clinical including Pharmacokinetic and Toxic kinetic study, and clinical including Bioavailability, Bioequivalence study. This are play significant role and help in improvement in technology and analytical methods. Recent years have witnessed the introduction of several high- quality review articles into the literature covering various scientific and technical aspects of bioanalysis. Method validation and development use for the purpose of suitability of method for their intended purpose, this are important in Drug Discovery and Development. It including a validation parameters are Accuracy, Precision, Range, Calibration Curve, Recovery, Limit of Detection, Limit of Quantitation, Specificity, Selectivity and Stability, Ruggedness. This applicable in bio analysis, FDA and EMA guidelines. There are 3 main Extraction techniques used in sample preparation in bioanalysis is precipitation, liquid –liquid extraction, solid phase extraction. Detection of analyte by using hyphenated and chromatographic techniques like LC-MS/MS, HPLC, GC-MS. This LC-MS/MS is commonly used in a bioanalysis. This bio analysis study used in Pharmaceutical, Biomedical research purpose. Many challenges in pharmaceutical industry that fulfill by the utilization of analytical technologies and high-throughput automated platforms has been employed; in order to perform more experiments in a shorter time frame with increased data quality.
生物样品中化学和生物药物及其代谢物的定量测量。这用于临床和非临床研究。非临床包括药代动力学和毒性动力学研究,临床包括生物利用度和生物等效性研究。这对技术和分析方法的改进起着重要的作用。近年来,文献中出现了几篇高质量的综述文章,涵盖了生物分析的各个科学和技术方面。方法验证和开发的目的是使方法适合其预期目的,这在药物发现和开发中很重要。它包括一个验证参数是准确度,精密度,范围,校准曲线,回收率,检出限,定量限,特异性,选择性和稳定性,坚固性。这适用于生物分析,FDA和EMA指南。生物分析中样品制备的萃取技术主要有沉淀法、液-液萃取法和固相萃取法。分析物的联用和色谱技术,如LC-MS/MS、HPLC、GC-MS等。本LC-MS/MS常用于生物分析。本生物分析研究用于制药、生物医学的研究目的。利用分析技术和高通量自动化平台来解决制药行业的许多挑战;为了在更短的时间内进行更多的实验,提高数据质量。
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引用次数: 5
Quality Evaluation of Generic Products of Metformin and Vildagliptin Tablets 二甲双胍和维格列汀片仿制药质量评价
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00043
Bhavana Habib, Jyoti Mittha
The aim of the present study was the evaluation and comparison between four different Metformin and Vildagliptin tablets which are commercially available in Indian market. These tablets were assessed for various pharmacopoeial quality control tests. Parameters including weight variation, hardness, friability, drug content, and disintegration time were evaluated. Results were within acceptable limits for all selected products (three generic and an innovator). These results show that the tested generic products were biopharmaceutically similar to the innovator formulation. Therefore, the consumer can select any one of these equivalent products as a substitute for innovator product in case of cost concern or unavailability.
本研究的目的是评价和比较在印度市场上可买到的四种不同的二甲双胍和维格列汀片。对这些片剂进行了各种药典质量控制试验。评价指标包括重量变化、硬度、脆度、药物含量、崩解时间等。所有选定产品的结果均在可接受范围内(三个仿制药和一个创新产品)。这些结果表明,测试的仿制产品在生物制药方面与创新配方相似。因此,消费者可以选择这些等效产品中的任何一种作为创新者产品的替代品,以防成本问题或不可用。
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引用次数: 1
Method Development and Validation for the Estimation of Etizolam and Propranolol Hydrochloride in bulk and Combined Dosage Forms by Simultaneous and Derivative Spectroscopic Methods 同时光谱法和导数光谱法测定盐酸安替唑仑和普萘洛尔原料药和复方药的含量
Pub Date : 2021-11-27 DOI: 10.52711/2231-5675.2021.00045
Susmeena Tabassum Kapatrala, Vinod Kumar Kondreddy, Swapna Kandlapalli, Tejaswi Male
Accurate, simple, sensitive and rapid economic UV spectroscopic methods were developed for the estimation of Etizolam and Propranolol Hydrochloride in bulk and combined dosage form. The present study deals with the UV spectroscopic method development and validation for the Simultaneous Equation method and First Derivative method of Etizolam and Propranolol Hydrochloride in bulk and combined dosage form at determined wavelength of Etizolam and Propranolol Hydrochloride at 244nm and 288nm for Simultaneous Equation method and 234nm and 289nm for First Derivative Method. The linearity range for Etizolam and Propranolol Hydrochloride was 1-5µg/ml and 10-50µg/ml, and exhibit good correlation coefficient of Etizolam and Propranolol Hydrochloride was 0.9877 and 0.9977 for Simultaneous Equation method and 0.9872 and 0.9977 for First Derivative method, respectively and excellent mean recovery (98-102%). The precision was found to be within limit (%RSD <2). Comparatively First Derivative method is more sensitive than Simultaneous Equation method. The methods were validated statistically and parameters like linearity, precision, accuracy, specificity and assay was studied according to ICH guidelines and can be applicable in determination of both drugs in routine quality control analysis of drugs in bulk and combined dosage form.
建立了一种准确、简便、灵敏、经济的紫外分光光度法测定盐酸安替唑仑和普萘洛尔原料药和复方药的含量。本研究对盐酸安替唑仑和普萘洛尔原厂剂型和复方剂型的紫外分光光度法进行了建立和验证,并对盐酸安替唑仑和普萘洛尔的联立方程法和一阶导数法在波长为244nm和288nm,一阶导数法在波长为234nm和289nm时进行了验证。安替唑仑与盐酸心得安的线性范围分别为1 ~ 5µg/ml和10 ~ 50µg/ml,联立方程法的相关系数分别为0.9877和0.9977,一阶导数法的相关系数分别为0.9872和0.9977,平均回收率为98 ~ 102%。精密度在限定范围内(%RSD <2)。相对而言,一阶导数法比联立方程法更灵敏。根据ICH指南对方法进行了统计验证,并对线性度、精密度、准确度、专属性、含量等参数进行了研究,可适用于原料药和复方制剂的常规质量控制分析。
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引用次数: 3
An Overview on Estimation of Lacidipine from Bulk and Formulation 拉西地平原料药和制剂评价综述
Pub Date : 2021-08-16 DOI: 10.52711/2231-5675.2021.00039
N. Dighe, Mayur Bhosale, Pallavi B. Gaikwad
Lacidipine is a calcium channel blocker used in treatment of cardiac arrhythmia. Several methods had been reported for the estimation of lacidipine from bulk and formulations. Here in this an attempt is made to summarize the different methods used along with their specifications. Every method reported for the analysis had its own advantages over the other methods. As per the industrial scalability HPLC is the most useful and effective method for the estimation of Lacidipine from bulk and formulations.
拉西地平是一种用于治疗心律失常的钙通道阻滞剂。已报道了几种从原料药和制剂中估计拉西地平的方法。在本文中,我们试图总结使用的不同方法及其规范。报告分析的每种方法都有其自身优于其他方法的优点。根据工业可扩展性,高效液相色谱法是测定拉西地平原料药和制剂中含量的最有效方法。
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引用次数: 0
Development and Validation of RP-HPLC Method for Determation of Acyclovir in Ointment 反相高效液相色谱法测定软膏中阿昔洛韦含量的建立与验证
Pub Date : 2021-08-16 DOI: 10.52711/2231-5675.2021.00035
Ajay B. Bedadurge, Kadare Mahesh, Vinod Matole, Parikshit D. Shirure, Sainath Suryawanshi, Ghodake Kajal
The analytical method was developed and validated for determination of acyclovir in ointment by High performance liquid chromatography. The separation was carried out on Luna C18 column (250 × 4.6mm × 5µ). The mobile phase consists of water: acetonitrile in the ratio 88:12 at flow rate 0.8ml/min with diode array detector wavelength at 254nm.The column temperature was adjusted at 30ºC±40ºC with injection volume 20µl.The retention time of acyclovir was 4.747min. The linearity of the calibration curve was linear over the concentration range 80-120µg/ml (r2=0.9996). The validation was carried out as per ICH guidelines. The development method was easy, rapid, linear, precise, accurate and consistent.
建立了高效液相色谱法测定软膏中阿昔洛韦的方法,并进行了验证。采用Luna C18色谱柱(250 × 4.6mm × 5µ)进行分离。流动相为水:乙腈,比为88:12,流速0.8ml/min,二极管阵列检测器波长254nm。柱温调节为30℃±40℃,进样量20µl。阿昔洛韦的保留时间为4.747min。在80 ~ 120µg/ml浓度范围内,校准曲线呈线性关系(r2=0.9996)。验证按照ICH指南进行。该方法简便、快速、线性、精密度、准确度、一致性好。
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引用次数: 1
Analytical Method Validation and Quantitative Analysis for Active Pharmaceutical Ingredient and Marketed Formulation of Teneligliptin Hydrobromide by UV Spectroscopy 氢溴酸替尼格列汀有效成分及市售制剂的紫外光谱分析方法验证及定量分析
Pub Date : 2021-08-16 DOI: 10.52711/2231-5675.2021.00034
Kalyani Farkade, M. Tawar
A Dipeptidyl peptidase-4 inhibitor teneligliptin hydrobromide is used for lowering blood glucose levels in people with diabetes mellitus. A very straight forward, quick, responsive and accurate UV- Spectrophotometric method of analysis have been developed for assessment of Teneligliptin Hydrobromide in pharmaceutical formulation. Since teneligliptin hydrobromide only absorbs UV in the low wavelength area, it cannot be identify with high sensitivity. Teneligliptin Hydrobromide has shown successful results for various analytical instruments only in the permutation of Taurine and Sodium periodate. The API was derivatives using Taurine and Sodium periodate in water and methanol. Drug exhibited distinct λmax in methanol at 281nm. Linearity was observed in the concentration range 10-80 μg/ml. The method was validated by recovery studies. The methods used are inexpensive and sensitive for the inference of teneligliptin hydrobromide in bulk drug and tablet dosage forms.
二肽基肽酶-4抑制剂氢溴替尼格列汀用于降低糖尿病患者的血糖水平。建立了一种简便、快速、灵敏、准确的盐酸替尼格列汀的紫外分光光度分析方法。由于氢溴化物替尼格列汀仅在低波长区域吸收紫外线,因此不能进行高灵敏度的鉴别。氢溴化替尼格列汀仅在牛磺酸和高碘酸钠的排列中显示出成功的结果。原料药是牛磺酸和高碘酸钠在水和甲醇中的衍生物。药物在281nm甲醇中表现出明显的λmax。在10 ~ 80 μg/ml浓度范围内呈线性关系。回收率研究证实了该方法的有效性。所采用的方法价格低廉,对氢溴替尼格列汀原料药和片剂剂型的推断灵敏。
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引用次数: 5
期刊
Asian Journal of Pharmaceutical Analysis
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