Simultaneous determination of calycosin‐7‐O‐β‐d‐glucoside,calycosin, formononetin,astragaloside IV and schisandrin in rat plasma by LC‐MS/MS: application to a pharmacokinetic study after oral administration of Shenqi Wuwei chewable tablets

A rapid, sensitive and reliable high‐performance liquid chromatography–mass spectrometry (LC‐MS/MS) method was developed and validated for simultaneous quantification of the five main bioactive components, calycosin, calycosin‐7‐O‐β‐d ‐glucoside, formononetin, astragaloside IV and schisandrin in rat plasma after oral administration of Shenqi Wuwei chewable tablets. Plasma samples were extracted using solid‐phase extraction separated on a CEC₁₈ column and detected by MS with an electrospray ionization interface in multiple‐reaction monitoring mode. Calibration curves offered linear ranges of two orders of magnitude with r > 0.995. The method had a lower limit of quantitation of 0.1, 0.02, 0.1, 1 and 0.1 ng/mL for calycosin, calycosin‐7‐O‐β‐d ‐glucoside, formononetin, astragaloside IV and schisandrin, respectively. Intra‐ and inter‐day precisions (relative standard deviation) for all analytes ranged from 0.97 to 7.63% and from 3.45 to 10.89%, respectively. This method was successfully applied to the pharmacokinetic study of the five compounds in rats after oral administration of Shenqi Wuwei chewable tablets. Copyright © 2014 John Wiley & Sons, Ltd.     

Formulation of Risperidone as Self-Nanoemulsifying Drug Delivery System in Form of Effervescent Tablets

Risperidone is an atypical antipsychotic drug used to treat schizophrenia. This study aims to formulate risperidone as effervescent tablets to improve patient compliance. Different nanoemulsion combinations were loaded with risperidone to improve its poor water solubility then adsorbed on Aeroperl. The formula showing highest drug dissolution was formulated as effervescent tablets. Factorial design was applied for different tablet formulation variables and the prepared formulae were tested for different criteria in comparison with their corresponding formulae containing drug without nanoemulsion formulation. Statistical analysis was used to determine the most desirable tablet formula considering its Carr index, effervescence time, and drug release.     

自动电位滴定法标定硫酸铈溶液和测定硫酸亚铁片中铁含量

采用自动电位滴定法标定硫酸铈溶液,并进行硫酸亚铁片中铁含量的测定。自动电位滴定法以电位突跃监测终点,在45℃~50℃之间,以草酸钠溶液标定硫酸铈溶液,测定值的相对标准偏差(n=5)为0.070%。取硫酸亚铁片1片用0.01mol·L-1硫酸溶液30mL溶解,直接用硫酸铈溶液滴定测定铁含量。方法用于硫酸亚铁片样品分析,回收率为100%,测定值的相对标准偏差(n=5)在1.2%~2.6%之间。     

解析电喷雾质谱法对感冒药中对乙酰氨基酚的快速检测

基于常压质谱的直接、快速、无需样品预处理检测的优势,该文拓展了其在药物质检领域的应用。采用自行搭建的解析电喷雾(DESI)装置,对常用感冒药对乙酰氨基酚片进行快速质谱检测,无需样品预处理,直接获得药片中有效成分的分子结构信息。为克服基质差异对定量分析的影响,以淀粉为基质构建对乙酰氨基酚模拟药片,在优化的基础上进行定量实验。针对实际药片中高浓度对乙酰氨基酚检测的需要,研究了其在较高浓度范围的定量关系,结果显示,方法对0.35~4.52 mg/mm^2范围内的对乙酰氨基酚具有较好的线性关系(r^2=0.9982),定量下限为1.903 ng/mm^2,检出限为0.237 ng/mm^2,加标回收率为102%~114%。对3种市售的对乙酰氨基酚片进行直接检测,与厂家提供的标准数据相比,相对标准偏差(RSD)为7.2%~12%,表明方法具有较好准确度。该工作很好地证明了DESI-MS在药品快检中的优势,从而为药品质检提供了潜在的高效、可靠的检测手段。     

Chemical Profile of Danning Tablets by LC-DAD Coupled with ESI-MS

HPLC-DAD coupled to an electrospray tandem mass spectrometer (ESI-MS) has been developed to analysis the chemical profile of Danning tablets. Separation was performed on a ZORBAX Extend C₁₈ analytical column by gradient elution with acetonitrile and formate buffer (containing 12.6 mmol L⁻¹ formic acid, adjusted to pH 5.0 with ammonia) at a flow rate of 0.8 mL⁻¹ min. Twenty-three peaks were identifies as the major compounds in this preparation. Similarity measurements of the HPLC-UV chromatograms were investigated by a Similarity Evaluation System for Chromatographic Fingerprinting of Traditional Chinese Medicine (TCM) in the range of 0.84–0.99, and principal components analysis (PCA) on the quantitative analysis data was further performed to evaluate the variation among batches. The proposed method gives chemical profiles of multi-components in one run, and therefore can be readily utilized as a comprehensive quality control approach for TCM.     

Monitoring the quality consistency of Weibizhi tablets by micellar electrokinetic chromatography fingerprints combined with multivariate statistical analyses,the simple quantified ratio fingerprint method,and the fingerprint–efficacy relationship

Micellar electrokinetic chromatography fingerprinting combined with quantification was successfully developed and applied to monitor the quality consistency of Weibizhi tablets, which is a classical compound preparation used to treat gastric ulcers. A background electrolyte composed of 57 mmol/L sodium borate, 21 mmol/L sodium dodecylsulfate and 100 mmol/L sodium hydroxide was used to separate compounds. To optimize capillary electrophoresis conditions, multivariate statistical analyses were applied. First, the most important factors influencing sample electrophoretic behavior were identified as background electrolyte concentrations. Then, a Box–Benhnken design response surface strategy using resolution index RF as an integrated response was set up to correlate factors with response. RF reflects the effective signal amount, resolution, and signal homogenization in an electropherogram, thus, it was regarded as an excellent indicator. In fingerprint assessments, simple quantified ratio fingerprint method was established for comprehensive quality discrimination of traditional Chinese medicines/herbal medicines from qualitative and quantitative perspectives, by which the quality of 27 samples from the same manufacturer were well differentiated. In addition, the fingerprint–efficacy relationship between fingerprints and antioxidant activities was established using partial least squares regression, which provided important medicinal efficacy information for quality control. The present study offered an efficient means for monitoring Weibizhi tablet quality consistency.     

Development of a method using high‐performance liquid chromatographic fingerprint and multi‐ingredients quantitative analysis for the quality control of Yangxinshi Pian

A simple and reliable method of high‐performance liquid chromatography with diode array detection method was developed for fingerprint analysis and simultaneous determination of six compounds including puerarin, salvianolic acid B, berberine hydrochloride, palmatine chloride, dehydrocorydaline, and icariin in the Chinese medicine preparation Yangxinshi Pian. The separation was performed on an Agilent Eclipse XDB‐C₁₈ reserved‐phase column (250 mm × 4.6mm I.D., 5 μm) using gradient elution with 50 mmol/L monopotassium phosphate aqueous solution and methanol as mobile phase at a flow rate of 1.0 mL/min. The column operating temperature was set at 30°C, and the detection wavelength was 280 nm. The method was validated by linearity, precision, accuracy, stability, and recovery. For fingerprint analysis, 25 peaks were selected as the common peaks, and four kinds of similarities including cosine similarity (S), ratio of similarity (S′), projection content similarity (C), and content similarity (P) were applied to evaluate the quality consistency of different batches of Yangxinshi Pian. The results showed that the developed method was an efficient tool for quality evaluation of Yangxinshi Pian.     

高效液相色谱法同时测定复方草珊瑚含片中四种活性成分

提出了高效液相色谱法同时测定复方草珊瑚含片中原儿荼酸、3-羟基-4-甲氧基苯甲酸、异嗪皮啶和迷迭香酸的含量。样品经甲醇超声提取,用Waters Sun Fire ODS色谱柱(4.6 mm×150mm,5μm)分离,以不同比例混合的乙腈和磷酸-水(0.1+99.9)溶液为流动相进行梯度洗脱,流量0.8mL·min~(-1),在294 nm波长处用紫外检测器检测。在优化的色谱条件下,4种活性成分可完全分离。原儿茶酸、3-羟基-4-甲氧基苯甲酸、异嗪皮啶和迷迭香酸的线性范围分别为2.508～50.16,18.40～368.0,6.375～127.5,41.04～820.8ng;平均回收率分别为92.8%,93.1%,91.9%,99.6%;相对标准偏差(n=6)均不大于5.0%。     

线性扫描极谱法测定消旋山莨菪碱

用线性扫描极谱法和循环伏安法研究了消旋山莨菪碱在0.3mol·L~(-1)磷酸氢二钠-磷酸二氢钾缓冲溶液(pH 6.70)中的电化学行为。消旋山莨菪碱于-1.095V(vs.SCE)处产生一灵敏的吸附波,消旋山莨菪碱质量浓度在0.10～10.0mg·L~(-1)范围内与其一次微分线性扫描峰电流i_p呈线性关系,检出限(3S/N)为0.06mg·L~(-1)。对5.0mg·L~(-1)消旋山莨菪碱溶液进行6次平行试验,相对标准偏差为0.34%,该方法用于片剂中消旋山莨菪碱含量的测定,测定值与标示值相符。