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Enhancement of Gum Solubility by Single Process of Humidification and Drying (Granulation) 湿干燥(造粒)单一工艺提高树胶溶解度
Pub Date : 2017-02-06 DOI: 10.4172/2153-2435.1000534
A. Sy, Nour Wf
Gum arabic is a complex, loose aggregate of sugars and hemicelluloses composed of Arabic acid nucleus connected with calcium, magnesium, potassium and sugars Arabinose, Galactose, and Rhamnose. It is found in mechanically ground or spray dried forms. The solubility varies between 2 h in the raw gum form and 20 min in spray dried form. This study tended to enhance the solubility by producing an instant soluble granulated form. The study was performed using atomized fluid bed drier. 50 kg of raw gum, subjected first to mechanical comminuting into powder, then treated with water by spraying at rate of 200 mL/min for 90 min. The inlet temperature was 70°C, and the outlet temperature was 40°C. The cabinet temperature was 40°C. Finally after water treatment process, the powder resized through Mesh size of 40 μm and the microbial test was done for the finished product. The solubility of the granulated instant soluble gum in room temperature was found to be less than 5 min compared to the spray dried form which is 20-30 min and 2 h for mechanical ground gum. The volume increased to three times compare to the mechanical form. It was concluded that granulation of gum under water spray significantly enhances the solubility and hence it is beneficial for uses in pharmaceutical technology. This study tended to produce a form of granulated gum which is easily soluble compared to the mechanically ground and spray dried forms.
阿拉伯胶是一种复杂、松散的糖和半纤维素的集合体,由阿拉伯酸核与钙、镁、钾和糖(阿拉伯糖、半乳糖和鼠李糖)连接而成。它以机械研磨或喷雾干燥的形式存在。其溶解度在生胶形式下为2小时,在喷雾干燥形式下为20分钟。本研究倾向于通过生产可溶的颗粒状来提高溶解度。研究采用雾化流化床干燥机进行。生胶50 kg,先机械粉碎成粉末,再以200 mL/min的速度喷水处理90 min,进口温度70℃,出口温度40℃。机柜温度为40℃。最后经水处理工艺后,对粉体进行粒径为40 μm的调整,并对成品进行微生物试验。颗粒状速溶胶在室温下的溶解度小于5分钟,而喷雾干燥形式的溶解度为20-30分钟,机械磨碎胶为2小时。体积增加到机械形式的三倍。结果表明,胶在水喷雾下造粒可显著提高胶的溶解度,有利于胶在制药工艺中的应用。与机械研磨和喷雾干燥的形式相比,本研究倾向于生产一种易于溶解的颗粒状口香糖。
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引用次数: 2
Stability-Indicating Chromatographic Methods for Determination of Agomelatine in Drug Substance and Drug Product 稳定性指示色谱法测定原料药和制剂中阿戈美拉汀的含量
Pub Date : 2017-01-31 DOI: 10.4172/2153-2435.1000531
M. Rizk, E. Taha, M. El-Alamin, Yasmin M. Sayed
Three sensitive and validated chromatographic methods were developed for determination of Agomelatine (AGO) in the presence of its degradation products in drug substance and drug product. The first and second methods were normal thin layer chromatographic (NP-TLC) and reversed phase thin layer chromatographic (RP-TLC) methods. Mobile phase consisting of ethyl acetate-ammonia (33%)-methanol (8.5:0.5:1, v/v/v) was used for NP-TLC while for RP-TLC using 0.1% triethylamine (TEA): acetonitrile (60:40 v/v) at pH=2. The chromatograms were scanned at 230 and 280 nm and determined in the range of 0.1-4 and 0.3-4 μg/spot with mean percentage recovery of 99.89 ± 1.141 and 100.01 ± 1.062 for NP-TLC and RP-TLC respectively. The third method was Micellar Liquid Chromatographic (MLC) method using C18 column and a mobile phase consisting of 0.1 M Sodium Dodecyl Sulphate (SDS), 15% butan-1-ol, 0.2% TEA in water adjusted to pH=3. The UV detection was achieved at 230 nm and determined in the range of 0.5-5 μg/mL with mean percentage recovery of 100.13 ± 0.970. The proposed methods were successfully applied as stability indicating methods under different stressed conditions according to the International Conference of Harmonization (ICH) guidelines. The methods showed good selectivity, repeatability, linearity and sensitivity according to the evaluation of the validation parameters.
建立了测定原料药和制剂中阿戈美拉汀(AGO)降解产物的三种灵敏、有效的色谱方法。第一、二种方法分别为正相薄层色谱法(NP-TLC)和反相薄层色谱法(RP-TLC)。NP-TLC采用醋酸乙酯-氨(33%)-甲醇(8.5:0.5:1,v/v/v)为流动相,RP-TLC采用0.1%三乙胺(TEA):乙腈(60:40 v/v)为流动相,pH=2。在230和280 nm处扫描,测定范围为0.1 ~ 4和0.3 ~ 4 μg/点,NP-TLC和RP-TLC的平均回收率分别为99.89±1.141和100.01±1.062。第三种方法是胶束液相色谱(MLC)法,采用C18色谱柱,流动相为0.1 M十二烷基硫酸钠(SDS)、15%丁醇、0.2% TEA,水溶液pH=3。紫外检测波长为230 nm,检测范围为0.5 ~ 5 μg/mL,平均回收率为100.13±0.970。根据国际协调会议(ICH)的指导方针,所提出的方法成功地作为不同应力条件下的稳定性指示方法应用。通过对验证参数的评价,该方法具有良好的选择性、重复性、线性和灵敏度。
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引用次数: 3
Preferential Solvation of Drugs in Binary Solvent Mixtures 药物在二元溶剂混合物中的优先溶剂化
Pub Date : 2017-01-23 DOI: 10.4172/2153-2435.1000537
Y. Marcus
The preferential solvation of many drugs in binary solvent mixtures, as derived by means of the quasi-lattice quasi-chemical and the inverse Kirkwood-Buff integrals methods from solubility and other thermodynamic data, is reviewed. The preferences were described in terms of the local mole fractions of the solvent components in the solvation sphere of the drug molecule and their differences with respect to these mole fractions in the bulk: the preferential solvation parameters. When data were available at several temperatures these preferences were described in terms of the enthalpic and entropic contributions.
从溶解度和其它热力学数据出发,利用准晶格准化学积分法和逆Kirkwood-Buff积分法推导出许多药物在二元溶剂混合物中的优先溶剂化。这些偏好是根据药物分子溶剂化球中溶剂组分的局部摩尔分数和它们相对于这些摩尔分数的差异来描述的:优先溶剂化参数。当有几个温度下的数据可用时,这些偏好用焓和熵的贡献来描述。
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引用次数: 72
Simultaneous Determination and Mutual Interaction Study of Ciprofloxacin and Chloramphenicol in Concomitant Administration by a New UPLC Method 新型高效液相色谱法同时测定环丙沙星与氯霉素的相互作用研究
Pub Date : 2017-01-23 DOI: 10.4172/2153-2435.1000535
M. Uddin, Suman Das, Mijan Nh, Al-amin, H. R. Bhuiyan
A new simple, fast, accurate, precise and reproducible UPLC method was developed for the simultaneous estimation of ciprofloxacin and chloramphenicol. Reversed-phase Shim-pack XR-ODS (100 × 3.0 mm, 1.7 μm) column was used to resolve the drugs utilizing a mixture of CH3OH and 5 mM NaH2PO4 as mobile phase at gradient program equilibrated initially by 56:44 (v/v). The mobile phase was pumped at a flow rate of 0.20 mL min-1 with detection at 280 nm. 10 μL volume of sample was injected by the auto sampler. Separation was completed within 3.82 ± 0.03 minutes. For both drugs linear was obtained over a studied concentration range of 10 μg mL-1 with correlation coefficient 0.999. Relative Standard Deviation (RSD) for intra and inter day precision was <1.5% indicating the method’s good reproducibility. The mean recovery of the drug determination was 99.39%. LOD was found to be 0.025, 0.020 μg mL-1 for ciprofloxacin and chloramphenicol, respectively. The proposed method might be applied for routine analysis of both drugs in bulk and pharmaceutical formulations. Furthermore, no experimental evidences in favour of adverse pharmaceutical interaction were revealed in their concomitant use.
建立了一种简便、快速、准确、精密度高、重复性好的高效液相色谱(UPLC)同时测定环丙沙星和氯霉素含量的方法。采用反相Shim-pack XR-ODS (100 × 3.0 mm, 1.7 μm)色谱柱,以CH3OH和5 mm NaH2PO4的混合物为流动相,梯度程序初始平衡为56:44 (v/v),进行药物分离。流动相以0.20 mL min-1的流速泵送,检测波长为280 nm。自动进样器进样量为10 μL。分离在3.82±0.03分钟内完成。两种药物在10 μg mL-1的浓度范围内均呈线性关系,相关系数为0.999。日内、日间精密度的相对标准偏差(RSD) <1.5%,重复性好。平均加样回收率为99.39%。环丙沙星和氯霉素的检出限分别为0.025、0.020 μ mL-1。所提出的方法可用于原料药和制剂的常规分析。此外,没有实验证据表明,有利于不良药物相互作用,在他们的共同使用被揭示。
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引用次数: 1
Spectrofluorimetric Estimation of Some Sulfhydryl – Containing Drugs by Demasking Reaction of the Palladium Chelate of 8-Hydroxyquinoline-5-Sulfonic Acid 8-羟基喹啉-5-磺酸钯螯合物掩膜反应荧光光谱法测定某些含巯基药物
Pub Date : 2017-01-13 DOI: 10.4172/2153-2435.1000532
Haggag Rs, Belal Sf, Hewala, ElRouby Oa
A simple and sensitive spectrofluorimetric method has been developed for the determination of some selected sulfhydryl–containing drugs namely Acetylcysteine (ACS), Captopril (CAP) and Mesna (MSN). The method is based on the interaction of the drugs with potassium (5-sulfoxino) palladium II in alkaline medium in presence of magnesium ions, where the sulfhydryl group combines with palladium from the non-fluorescent potassium bis (5-sulfoxino) palladium II. The resulting 8-hydroxy-5-quinoline sulfonic acid coordinates with magnesium to form the fluorescent chelate that is a measure of the amount of sulfhydrl containing drug analyzed. The fluorescence intensity was measured at an emission wavelength of 485 nm, by excitation at 345 nm. All the experimental parameters affecting the reaction were studied and optimized. The proposed method was applicable over the concentration range of 0.04-0.44 μg/mL for the three drugs and was applied for their determination in bulk form and in pharmaceutical preparations without interference from common excipients. The assay results were statistically compared with those obtained from previously reported methods where no significant difference was found between them. The selectivity and the stability-indicating aspect of the proposed method were confirmed by preparing the disulphides of the studied drugs and applying the reaction to the parent drugs in presence of their disulphides where no interference was detected from these related substances. By virtue of its high sensitivity, the proposed method was also extended to analyze the drugs in spiked human plasma and urine.
建立了一种简单、灵敏的含巯基药物乙酰半胱氨酸(ACS)、卡托普利(CAP)和美斯那(MSN)的荧光光谱测定方法。该方法是基于药物与钾(5-亚砜)钯II在镁离子存在的碱性介质中的相互作用,其中巯基与非荧光双(5-亚砜)钯II中的钯结合。由此产生的8-羟基-5-喹啉磺酸与镁配合形成荧光螯合物,这是对含巯基药物分析量的测量。在发射波长为485 nm,激发波长为345 nm处测量荧光强度。对影响反应的实验参数进行了研究和优化。该方法适用于3种药物在0.04 ~ 0.44 μg/mL的浓度范围内,适用于原料药和制剂中三种药物的测定,不受常用辅料的干扰。测定结果与以前报道的方法进行了统计比较,发现它们之间没有显着差异。通过制备所研究药物的二硫化物,并在母体药物的二硫化物存在的情况下将反应应用于母体药物,并且没有检测到这些相关物质的干扰,从而证实了所提出方法的选择性和稳定性。该方法具有较高的灵敏度,可应用于人血浆和尿液中药物的分析。
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引用次数: 1
Fabrication of Surgical Sutures Coated with Curcumin Loaded Gold Nanoparticles 姜黄素载金纳米颗粒包被手术缝合线的制备
Pub Date : 2017-01-09 DOI: 10.4172/2153-2435.1000529
S. Sunitha, K. Adinarayana, T. Pankaj, P. SravanthiReddy, G. Sonia, R. Nagarjun, C. VeerabhadraSwamy, D. Sujatha
Sutures are biomaterials regarded as a major cause of Surgical Site Infections (SSIs). Present work aims at a novel strategy to reduce nosocomial infections by coating sutures with antimicrobial drugs. Gold Nanoparticles (GNPs) coated with antimicrobial drugs are well known for their antimicrobial activity. Hence, synthesis of gold nanoparticles by chemical reduction method followed by preparation of curcumin pegylated GNPs (CPGNPs) were carried out. The formation of the gold nanoparticles, thiolated gold nanoparticles (PGNPs) and CPGNPs was characterized by UV-Vis absorption spectroscopy, Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM) techniques. The average particle size and polydispersity index of drug conjugated gold NPs were found to be 147.8 nm ± 2.03 nm and 0.286 respectively. The plain sutures (purchased from local market) were coated with curcumin pegylated GNPs by dipping technique and characterized by SEM to ensure the coating of curcumin conjugated gold nanoparticles on plain sutures. The CPGNPs coated sutures were evaluated for mechanical properties, drug release studies, biocompatibility, haemo-compatibility, sensitization and for in vivo studies. Histopathology was also done to study the effect of coated sutures on inflammation and cell repair at the site of surgery. The optimized coated sutures exhibited sustained drug release for 4 days and the antibacterial activity of the coated sutures was noticed in comparison to the uncoated sutures. From in vivo studies, it was clearly evident that coated sutures healed the tissue much faster than the uncoated sutures and less inflammation was observed. The same was concluded by the histopathology reports. The successful designing and development of drug-coated biodegradable sutures highlight the applicability of novel technique of coating for effective reduction of SSIs during the hospital stay.
缝合线是一种生物材料,被认为是手术部位感染的主要原因。目前的工作旨在一种新的策略,以减少医院感染涂层缝合线与抗菌药物。包裹有抗菌药物的金纳米颗粒(GNPs)因其抗菌活性而闻名。因此,采用化学还原法制备了金纳米粒子,然后制备了姜黄素聚乙二醇化GNPs (CPGNPs)。利用紫外可见吸收光谱、傅里叶变换红外光谱(FT-IR)和扫描电子显微镜(SEM)技术对金纳米粒子、硫代金纳米粒子(PGNPs)和CPGNPs的形成进行了表征。药物偶联金纳米粒子的平均粒径为147.8 nm±2.03 nm,多分散性指数为0.286。通过浸渍技术将从当地市场购买的平缝线涂覆姜黄素聚乙二醇化GNPs,并通过扫描电镜对其进行表征,以确保姜黄素共轭金纳米颗粒在平缝线上的涂覆。对CPGNPs包被缝合线的力学性能、药物释放研究、生物相容性、血液相容性、致敏性和体内研究进行评估。组织病理学还研究了包覆缝线对手术部位炎症和细胞修复的影响。优化后的包被缝线具有4 d的药物持续释放,且包被缝线的抗菌活性明显高于未包被缝线。从体内研究中可以清楚地看出,包覆缝合线比未包覆缝合线愈合组织的速度要快得多,并且观察到的炎症较少。组织病理学报告也得出同样的结论。药物涂层生物可降解缝合线的成功设计和开发,突出了新型涂层技术在有效减少住院期间ssi的适用性。
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引用次数: 6
Characterization and Aldose Reductase Inhibitory Effect of Carica papaya Extract 番木瓜提取物的表征及醛糖还原酶抑制作用
Pub Date : 2017-01-01 DOI: 10.4172/2153-2435.1000576
E. Adewole
Objective and aim: the aim of the research work was to characterize the methanolic extract of C. papaya and then carried out the anti-diabetic inhibitory potential of the extract against Aldose Reductase enzymes.Materials and methodology: The C. papaya leaves were harvested fresh and air dried for five days at room temperature and blended into powdered form using electric blender. It was subsequently subjected to extraction using analytical grade of methanol solvent. Enzymatic reaction assays were performed using standard recommended protocol with slight modifications and the extract was characterized using Gc-Ms. Finally some of the identified compounds were screened for various degrees of drug characteristics using Online OSIRIS property explorer.Results: the IC50 value (1.22 ± 0.63 μg/mL) of ALR1 was better than the standard vaproic acid of IC50 (57.4 ± 10 μg/mL) and the IC50 (1.22+0.06 μg/mL) of ALR2 of the methanolic extract was better than the sorbinil standard IC50 (3.10 ± 0.20 μg/mL). The promising inhibitory aldose reductase may be due to the compounds present in the methanolic extract and these compounds include; phytol, Oxalic acid,6-ethyloct-3-yl isobutyl ester, 3,methyl-2-(2- oxopropyl)Furan, Carbonic acid, isobutyl undec-10-enyl ester, D-mannitol,1 decylsulfonyl and 1H-Imidazole,1(1- oxooctadecyl), these identified compounds possess different drug characteristics such as, solubility, mutagenic, irritability, H-bond acceptor and H-bond donor.Conclusion: The promising potent inhibitory activity of C. papaya showed that the plant leaves could be further researched into as alternative for resolving cataract eye problem associated with prolongs diabetes mellitus.
目的与目的:研究木瓜醇提物对醛糖还原酶(al糖还原酶)的抑制作用。材料与方法:新鲜收获木瓜叶,室温风干5天,用电动搅拌机混合成粉末状。随后用分析级甲醇溶剂进行萃取。酶促反应试验采用标准推荐方案,稍作修改,提取物采用Gc-Ms表征。最后利用在线OSIRIS属性探索者对鉴定出的部分化合物进行不同程度的药物特性筛选。结果:ALR1的IC50值(1.22±0.63 μg/mL)优于标准丙戊酸的IC50值(57.4±10 μg/mL),甲醇提取物ALR2的IC50值(1.22+0.06 μg/mL)优于山梨醇标准IC50值(3.10±0.20 μg/mL)。有希望的抑制性醛糖还原酶可能是由于甲醇提取物中存在的化合物,这些化合物包括;叶绿醇、草酸、6-乙基-3-基异丁基酯、3、甲基-2-(2-氧丙基)呋喃、碳酸、异丁基十一-10-烯基酯、d -甘露醇、1-癸基磺酰基和1h -咪唑、1(1-氧辛基),这些已鉴定的化合物具有不同的药物特性,如溶解度、诱变性、过敏性、氢键受体和氢键供体。结论:木瓜叶具有良好的抗糖尿病活性,可进一步研究其作为治疗慢性糖尿病伴白内障眼病的替代药物。
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引用次数: 3
Development and Validation of Spectrophotometric and Spectrofluorimetric Methods for the Determination of Cyclobenzaprine HCl 分光光度法和荧光光度法测定盐酸环苯扎林的方法建立与验证
Pub Date : 2017-01-01 DOI: 10.4172/2153-2435.1000574
Nesrin K. Ramadan, Mohamed Ta, Fouad Rm, Ala-Eddin Al Moustafa
Five simple and sensitive methods were developed for the determination of cyclobenzapirine hcl (CB) in presence of its degradation product anthraquinone (AQ). Method A dual wavelength spectrophotometry (DW); where two wavelengths were selected for the drug 283 and 306 nm in such a way that the difference in absorbance was zero for its degradation. Method B ratio difference spectrophotometry (RD) was depended on measuring the ratio difference between 290 and 305 nm. Method C was depended on measuring the peak amplitude of the first derivative of the ratio spectra (1DD) at 282 and 306 nm. Method D Isoabsorptive Point (ISO) at 280 nm Coupled with Second Derivative (2D). Method E depending on spectrofluorimetric determination of cyclobenzapirine HCl through quenching of uranyl acetate with ʎexi 228 nm and ʎem at 458 nm. Linearties were obtained in concentration range 5 μg/ml – 30 μg/ml in case of methods A, B, C and D, while in case of methods E linearity was obtained in concentration range of 1 μg/ml –10 μg/ml. The five methods were found to be specific for CB in presence of different concentration % of its degradation product. The five proposed methods were successfully applied for the determination of CB in Multirelax tablets. Statistical comparison between the results obtained by the proposed methods and that obtained by the official one for the determination of the drug was done, founding that there were no significant differences between them.
建立了5种简便、灵敏的测定环苄吡林盐酸(CB)降解产物蒽醌(AQ)含量的方法。方法采用双波长分光光度法;其中为药物选择了两个波长283 nm和306 nm,以使其降解的吸光度差异为零。方法采用B比差分光光度法(RD)测定290 ~ 305 nm之间的比差。方法C是测定比值光谱(1DD)一阶导数在282和306 nm处的峰值振幅。方法D: 280 nm处等吸收点(ISO)与二阶导数(2D)耦合。方法:采用醋酸铀酰在228 nm和458 nm淬灭光度法测定盐酸环benzapirine的含量。方法A、B、C、D在5 μg/ml ~ 30 μg/ml浓度范围内呈线性,方法E在1 μg/ml ~ 10 μg/ml浓度范围内呈线性。结果表明,在不同浓度的降解产物存在的情况下,这五种方法都具有特异性。五种方法均可用于多舒片中邻苯二甲酸乙酯的含量测定。将所提出的方法与官方药物测定方法进行了统计比较,发现两者之间没有显著差异。
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引用次数: 1
Validated Stability-Indicating UPLC Method for Determination of Dapoxetine and Fluoxetine: Characterization of Their Hydrolytic Degradation Products, Kinetic Study and Application in Pharmaceutical Dosage Forms 稳定性指示高效液相色谱法测定达泊西汀和氟西汀:水解降解产物表征、动力学研究及其在制剂中的应用
Pub Date : 2017-01-01 DOI: 10.4172/2153-2435.1000571
S. M. Soliman, H. M. El-Agizy, A. E. Bayoumi
New isocratic stability-indicating reversed phase UPLC method was developed for determination of two antidepressant drugs dapoxetine hydrochloride (DAP) and fluoxetine hydrochloride (FLX) in the presence of their hydrolytic degradation products namely; (+)-N, N-dimethyl-1-phenyl-3-propanolamine (DAP Deg I), N-methyl- 3-hydroxy-3-phenyl propyl amine (FLX DegI), α, α, α-Trifluorotoluene (FLX Deg II) and application in their pharmaceutical dosage forms. UPLC method using small sub-1.8 μm particle was developed for separation and determination of the selected drugs using Agilent Eclipse XDB C18 (50 mm x 2.1 mm i.d., 1.8 μm) column. Upon using UPLC, the run time could be reduced 5-fold and the solvents consumption decreased 10 tims. Quantification is achieved by detection wavelength at 210 nm, based on peak area. The linear ranges were 0.05-100 μg/mL and 0.30-100 μg/mL with LOD of 0.01 and 0.09 μg mL-1 and mean recoveries of 99.41 ± 1.02 and 100.05 ± 0.89 for DAPand FLX, respectively, the developed method was successfully applied to analysis of DAP and FLX in bulk powder, laboratory-prepared mixtures containing different percentages of degradation products and pharmaceutical dosage forms. UPLC method was also directed to investigate the degradation kinetic processes of both drugs. It was followed pseudo-first order reactions with a degradation reaction rate constant (k) of 0.0575 (h-1) and 0.965 (h-1) and half-life (t1/2) of 12.04 and 0.75 (h) for DAP and FLX, respectively. The degradation rate (k) obeyed Arrhenius equation and the activation energies were calculated. The degradation products (I-III) were separated by UPLC and subjected to MS spectrometry to confirm their structures and elucidate degradation pathway. The developed methods were validated as per ICH guidelines.
建立了抗抑郁药盐酸达泊西汀(DAP)和盐酸氟西汀(FLX)在水解降解产物存在下的测定方法。(+)- n, n -二甲基-1-苯基-3-丙醇胺(DAP DegI), n -甲基-3-羟基-3-苯基丙胺(FLX DegI), α, α, α-三氟甲苯(FLX Deg II)及其在药用剂型中的应用。采用Agilent Eclipse XDB C18 (50 mm x 2.1 mm id, 1.8 μm)色谱柱,建立亚1.8 μm小颗粒超高效液相色谱法对所选药物进行分离和测定。使用UPLC后,运行时间缩短了5倍,溶剂消耗减少了10倍。根据峰面积,通过210 nm的检测波长实现定量。该方法在0.05 ~ 100 μg/mL和0.30 ~ 100 μg/mL的线性范围内,检出限分别为0.01和0.09 μg mL-1,平均回收率分别为99.41±1.02和100.05±0.89。该方法成功地应用于粉末、不同降解产物百分比的实验室配制混合物和药物剂型中DAP和FLX的分析。采用超高效液相色谱法研究了两种药物的降解动力学过程。对DAP和FLX进行伪一级反应,降解速率常数(k)分别为0.0575 (h-1)和0.965 (h-1),半衰期(t1/2)分别为12.04和0.75 (h)。降解速率k符合Arrhenius方程,并计算活化能。降解产物(I-III)经UPLC分离,质谱分析确定其结构并阐明降解途径。根据ICH指南对开发的方法进行了验证。
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引用次数: 0
Speciation and Determination of Ionic and Trace-Level Colloidal Silver in Selected Personal Care Products by Thermal Lens Spectrometry 热透镜光谱法测定个人护理产品中离子和痕量胶体银的形态
Pub Date : 2017-01-01 DOI: 10.4172/2153-2435.1000573
D. Korte, A. Grahovac, Andrej Jerkič, O. Vajdle, J. Anojčić, Guzsvány, B. Budic, M. Franko
The collinear dual beam thermal lens spectrometric (TLS) detection in batch mode (BM), as well as combined with the flow injection analysis (FIA), was applied to determine the colloidal silver in personal care products available in the public pharmacies and declared by producers to contain nanosilver at the level of 5-30 μg ml-1. It was found, that the examined samples contain mainly ionic silver (99% or more), whereas the colloidal form of silver is at the level of less than 1 μg ml-1. The TLS methods were confirmed to be fast, precise, highly accurate and highly sensitive with limits of quantitation of 0.30 ng ml-1 and 1.50 ng ml-1 and relative standard deviations not higher than 1.2% and 6.0% for BM- and FIA-TLS configuration, respectively. The developed TLS methods have nearly 60 times lower LOQ values concerning the colloidal silver determination than the classical spectrophotometric method. To verify the obtained results of the real sample analysis the total amount of ionic silver was determined by the use of ICP-OES technique.
采用共线双光束热透镜光谱法(TLS)批量检测,并结合流动注射分析法(FIA),对公共药店销售的个人护理用品中纳米银的含量进行了检测,检测的纳米银含量为5 ~ 30 μg ml-1。结果发现,检测样品中离子银的含量主要在99%以上,而胶体银的含量低于1 μg ml-1。验证了TLS方法快速、精确、高准确度和高灵敏度,BM-和FIA-TLS配置的定量限分别为0.30 ng ml-1和1.50 ng ml-1,相对标准偏差分别不高于1.2%和6.0%。与传统的分光光度法相比,该方法测定胶体银的定量限降低了近60倍。为了验证实际样品分析的结果,用ICP-OES技术测定了离子银的总量。
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引用次数: 2
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Pharmaceutica Analytica Acta
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