离子色谱法测定复方卡托普利片中卡托普利和氢氯噻嗪的含量

建立离子色谱法测定复方卡托普利片中卡托普利和氢氯噻嗪含量的方法。在色谱柱为IonPacSCS1(4mm×250mm),保护柱为IonPacSCG1(4mm×50mm),淋洗液为甲烷磺酸(4mmol/L)+乙腈(26%),流速1.0mL/min,柱温35℃,进样量7μL,紫外检测波长215nm的条件下,测定结果表明,卡托普利和氢氯噻嗪在0.5～25μg/mL范围内线性关系良好,相关系数r分别为0.9997、0.9999,回收率分别为98.11%、94.24%。方法操作简单,灵敏度高、准确、重现性好,可用于复方卡托普利片的质量控制。     

In vivo Antimalarial Activity of Andrographis Paniculata Tablets

The formulation of three phytopharmaceutical products of Andrographispaniculata fractions (AP fraction A and B) containing diterpene lactones as an active substance were developed and their antimalarial activities against Plasmodium bergheihas been examined. In vivo antimalarial assay on P. berghei infected mice was carried out by oral administration,twice a dayfor four consecutive days of the AP fractions product, which were Tablet I: wet granulated formula of AP fraction A; Tablet II: wet granulated formula of AP fraction B; Tablet III: solid dispersion formula of AP fraction B.. The results revealed that three phytopharmaceutical products of A.paniculata were inhibited parasite's growth with inhibition range of 70.15% to 80.35%. There was no significant difference of antimalarial activities between Tablet II and III, meanwhile there was significant difference among Tablet I with Tablet II and Tablet III.It was concluded that antimalarial activity depending on raw material form of A. paniculata active substance.     

Determination of ticagrelol in rat plasma and tablets by micellar electrokinetic chromatography coupled with large volume sample stacking: Application to a pharmacokinetic study

A method using micellar electrokinetic chromatography coupled with large-volume sample stacking for the determination of ticagrelol was developed and validated. The analysis was performed in a fused silica capillary (41.5 cm effective length, 50 μm diameter) with ultraviolet detection at 195 nm. The background electrolytes were 30 mM phosphate buffer of pH 3.0 with 120 mM sodium dodecylsulfate and 10 % (v/v) acetonitrile (120 s X 50 mbar; 20°C; -18 kV) and 30 mM borate buffer of pH 8.5 with 75 mM sodium dodecylsulfate (120 s X 50 mbar; 20°C; 25 kV); under acidic and alkaline conditions, respectively. The method was found to be reliable with respect to specificity, linearity of the calibration line (R² > 0.99), repeatability (relative standard deviation 2.56%–3.34%), and accuracy (recovery in the range 101.21%–102.67%). The limits of detection and quantitation were 0.032, 0.071, and 0.087, 0.188 μg/mL, respectively. The method was successfully applied for the determination of ticagrelol concentrations in rat plasma and tablets with good recoveries and reproducibility. The presented method proved to be suitable for monitoring ticagrelor in rat plasma.     

D1-Differential Potentiometric and 1H-NMR Spectrometric Determinations of Ketoconazole and its Formulations

Abstract

Two rapid and direct quantitative assays have been investigated for ketoconazole alone and in tablet form. the first one is a non-aqueous potentiometric titration in which the equivalence point has been located graphically using its distinct and sharp D₁differential (peak-shape) potentiograph. the second is based on ₁H-NMR spectrometry and involves the integration of the methyl protons-signal of ketoconazole (at 2.07 δ) relative to that of benzocaine (at 1.30 δ) which is used as internal standard. the obtained results were in good agreement with regard to accuracy, precision as well as sensitivity and reproducibility. However, by comparison with the official USP procedure, the two methods were significantly more accurate and more sensitive. the validity of the two methods were confirmed using the authentic addition technique.     

膜富集-可见漫反射光谱法测定池塘水和维生素B_(12)药片中痕量钴

1-(2-吡啶偶氮)-2-萘酚与钴离子生成暗绿色的络合物,反应后将其过滤到膜上,测得膜表面漫反射光谱,据此提出了膜富集-可见漫反射光谱法测定池塘水和维生素B12药片中痕量钴的方法。钴的质量浓度在0.2~3.0μg·L-1和3.0~10.0μg·L-1范围内与其吸光度呈线性关系,检出限(3s/k)为0.093μg·L-1。方法用于池塘水和维生素B12药片的分析,加标回收率在96.7%~105%之间,测定值的相对标准偏差在1.4%~2.9%之间。     

NMR data visualization,processing, and analysis on mobile devices

Touch‐screen computers are emerging as a popular platform for many applications, including those in chemistry and analytical sciences. In this work, we present our implementation of a new NMR ‘app’ designed for hand‐held and portable touch‐controlled devices, such as smartphones and tablets. It features a flexible architecture formed by a powerful NMR processing and analysis kernel and an intuitive user interface that makes full use of the smart devices haptic capabilities. Routine 1D and 2D NMR spectra acquired in most NMR instruments can be processed in a fully unattended way. More advanced experiments such as non‐uniform sampled NMR spectra are also supported through a very efficient parallelized Modified Iterative Soft Thresholding algorithm. Specific technical development features as well as the overall feasibility of using NMR software apps will also be discussed. All aspects considered the functionalities of the app allowing it to work as a stand‐alone tool or as a ‘companion’ to more advanced desktop applications such as Mnova NMR. Copyright © 2015 John Wiley & Sons, Ltd.     

High‐Throughput Synthetic Chemistry Enabled by Organic Solvent Disintegrating Tablet

Synthetic chemistry remains a time‐ and labor‐intensive process of inherent hazardous nature. Our organic solvent disintegrating tablet (O‐Tab) technology has shown potential to make industrial/synthetic chemistry more efficient. As is the case with pharmaceutical tablets, our reagent‐containing O‐Tabs are mechanically strong, but disintegrate rapidly when in contact with reaction media (organic solvents). For O‐Tabs containing sensitive chemicals, they can be further coated to insulate them from air and moisture.     

Comparison of infrared attenuated total reflection and Raman spectroscopy in the quantitative analysis of diclofenac sodium in tablets

The quantification of diclofenac sodium (DS) in tablets was performed using partial least squares (PLS) models based on FTIR ATR (Fourier transform infrared attenuated total reflection) and FT-Raman spectra. Separate calibration models were built for two groups of tablets, standard and sustained release, containing different excipients. To compare the predictive ability of these models the relative standard errors of prediction (RSEP) were calculated. In the case of DS determination from the Raman data, RSEP error values in the range of 2.4-2.8% (2.7-2.9%) for the calibration (validation) data sets were obtained. For ATR models constructed using spectra registered three times for each sample, RSEP errors in the range of 3.6-3.7% (4.2-4.3%) were found. These errors decreased to 2.8% (3.0%) when spectra collected six times were applied. Five commercial products containing 25, 50, 75 and 100 mg of DS per tablet were quantified. Concentrations derived from the elaborated models correlated strongly with the results of reference analyses and gave recoveries of 99.1-101.3% and 99.1-101.7% for the ATR and Raman data, respectively. Although both spectroscopic techniques can be used as fast and convenient alternatives to the standard pharmacopeial methods of DS quantification in solid dosage forms, in the case of the ATR technique, it is necessary to repeat measurements at least a few times to obtain acceptable quantification errors.     

Simultaneous determination of ibuprofen and paracetamol using derivatives of the ratio spectra method

Simple, rapid and accurate new method is described for the simultaneous determination of ibuprofen (IB) and paracetamol (PA) in two components mixture and Cetofen tablets. The method depends on the derivative of the ratio spectra DD by measurement of the amplitude of ¹DD at 225.6 nm and the amplitude of ²DD at 238.9 nm for IB and PA. Calibration graphs are linear in the range 2–32 (LOD 0.53) and 2–24 (LOD 0.57) μg/ml IB and PA, respectively. The proposed method is successfully applied for simultaneous determining IB and PA in authentic mixtures and Cetofen tablets.     

胶束电动毛细管色谱法测定消糖灵中的优降糖

 以甲氧苄氨嘧啶为内标,采用胶束电动毛细管色谱法分离测定了新药消糖灵中的优降糖。电泳条件：以25 mmol/L硼砂-30 mmol/L十二烷基硫酸钠（pH 9.0）为电泳介质,未涂层石英毛细管（50 μm i.d.×39.5 cm,有效分离长度34.8 cm）为分离通道,压力进样(68.95 kPa.s),17 kV恒压电泳（28 ℃）,检测波长228 nm。优降糖在14 min内与其他成分得到很好分离,且质量浓度为25 mg/L～275 mg/L时,优降糖可进行定量分析,加标回收率为(100.6±1.4)%。方法简便、快速,结果准确,重现性好,可用于优降糖复方制剂的质量控制。