A comparative pharmacokinetic study of three flavonoids and three anthraquinones in normal and gastrointestinal motility disorders rat plasma after the oral administration of Wei‐Chang‐Shu tablet using high‐performance liquid chromatography–tandem mass spectrometry

A simple, fast and reliable high‐performance liquid chromatography–tandem mass spectrometry method was developed and validated for the simultaneous quantification and pharmacokinetic study of three flavonoids (liquiritigenin, isoliquiritigenin and formononetin) and three anthraquinones (emodin, rhein and aloe‐emodin), which are the bioactive ingredients of Wei‐Chang‐Shu tablet found in rat plasma. After extraction by liquid–liquid extraction with ethyl acetate, chromatographic separation was achieved on an Agilent Zorbax SB‐C₁₈ column (4.6 × 150 mm, 5 μm) at a flow rate of 1 mL/min by gradient elution using 0.1% aqueous acetic acid and acetonitrile. The detection was performed using a triple quadrupole mass spectrometer equipped with electrospray ionization source in the negative ionization and selected reaction monitoring mode. Method validation was performed in terms of specificity, carryover, linearity (r > 0.99), intra−/inter‐day precision (1.0–10.1%), accuracy (relative error, <7.6%), stability (0.6–13.2%), extract recovery (74.9–91.9%) and matrix effect (89.1–109%). The lower limits of quantification of the six analytes varied from 0.92 to 10.4 ng/mL. The validated method was successfully applied to compare the pharmacokinetic properties of Wei‐Chang‐Shu tablet in normal rats and in rats with gastrointestinal motility disorders. The results indicated that there were obvious differences in the pharmacokinetic behavior between normal and model rats. This study will be helpful in the clinical application of Wei‐Chang‐Shu tablet.     

Tb3+敏化化学发光法测定氟罗沙星

利用Tb3+能大大增强Ce*$-H2SO3-FLX的化学发光,建立了一种简单、快速、高灵敏度、高选择性的测定氟罗沙星的新方法,氟罗沙星浓度在2.0×10-9～8.0×10-8 mol/L范围内时,发光强度与氟罗沙星浓度呈良好的线性关系,方法的检出限为8.3×10-10 mol/L,对2.0×10-8 mol/L的氟罗沙星平行测定11次,相对标准偏差为1.2%.并用该方法测定了沃尔得及天方片剂中氟罗沙星的含量,不经任何预处理,直接测定了尿样中氟罗沙星的含量及回收率,结果令人满意.     

富锌排铅咀嚼片临床排铅效果研究

采用自身对照及组间对照法,对富锌排铅咀嚼片(RZLR)进行了临床排铅效果研究。将60例高血铅试食者随机分成试食组和对照组,每组3 0例,试食组口服RZLR片,对照组口服安慰剂。口服一个月后,试食者乏力、头晕、失眠、关节痛等主要症状有较好的改善,血红蛋白、红细胞、白细胞、血清总蛋白、白蛋白、谷草转氨酶、谷丙转氨酶、尿素氮、肌酐及尿常规等各项临床检验指标均在正常范围,血铅下降81 5 μg/L ,尿铅排出增加1 6 0 μg/L ,两组比较有显著性差异(P <0 0 0 1 ) ,说明RZLR片对试食者身体健康无不良影响,有促进人体排铅作用     

Qualitative and quantitative analysis of the major constituents in Jin‐Mu‐Gan‐Mao tablet by high‐performance liquid chromatography with diode‐array detection and quadrupole time‐of‐flight tandem mass spectrometry

Jin‐Mu‐Gan‐Mao tablet is a well‐known traditional Chinese medicinal preparation, which has been used to treat the common cold in China. In this study, a systematic method was established for the qualitative and quantitative analysis of the major constituents in Jin‐Mu‐Gan‐Mao tablet. First, a method of high‐performance liquid chromatography with diode‐array detection and quadrupole time‐of‐flight mass spectrometry was developed for identification of the multi‐constituents. Thirty‐one compounds including ten phenolic acids, 18 flavonoids, and three iridoid glycosides were clearly identified by comparison with the reference standards, and 11 compounds were deduced by comparison with the literature data. Second, a new quantitative analysis method of Jin‐Mu‐Gan‐Mao tablet was established by high‐performance liquid chromatography with diode‐array detection. Twelve compounds, either with high contents or strong bioactivities, were chosen as marker components. This analytical method was validated through intra‐ and interday precision, repeatability, and stability, with respective relative standard deviations less than 1.74, 2.54, 2.44, and 2.48%. The limits of detection and quantification were less than 0.327 and 0.881 μg/mL, respectively. The overall recoveries ranged from 97.04–102.76% (relative standard deviation ≤ 2.91%). Then this validated method was applied to determine ten batches of Jin‐Mu‐Gan‐Mao tablet. The results indicated that these new approaches can be applicable for the qualitative and quantitative analysis of Jin‐Mu‐Gan‐Mao tablet.     

测量复方药物溶出度的全自动药物溶出度测定仪

自行设计组装了一套可以同时测定复方药剂的全自动药物溶出度测定仪。该仪器由光学检测系统（由光源、流动型吸收池，小型光谱仪组成）、自动进样系统、控制与数据处理系统和机械搅拌系统4部分组成。光学系统的检测器是线阵电荷耦合器件（CCD），故可进行同时全光谱采集。数据处理部分采用了自行设计的基于径向基函数的人工神经网络进行浓度预测。用本装置对市售复方药剂鲁南贝特进行的溶出度测量表明，测量的精密度高，准确度较高，分析速度快，样品无需前处理。     

Determination of flurbiprofen in pharmaceutical preparations by GC–MS

This article describes a gas chromatography–mass spectrometry (GC–MS) method for the determination of flurbiprofen in pharmaceutical preparations. The method is based on the derivatization of flurbiprofen with N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA). For GC–MS, electron ionization mode (EI = 70 eV) and selected ion monitoring (SIM) mode were used for quantitative analysis (m/z 180 for flurbiprofen). Calibration curve was linear between the concentration range of 0.25–5.0 μg/mL. Intra- and inter-day precision values for flurbiprofen were less than 3.64, and accuracy (relative error) was better than 2.67%. The mean recovery of flurbiprofen was 99.4% for pharmaceutical preparations. The limits of detection and quantification of flurbiprofen were 0.05 and 0.15 μg/mL, respectively. No interference was found from tablet excipients at the selected assay conditions. Also, the method was applied for the quality control of five commercial flurbiprofen dosage forms to quantify the drug and to check the formulation content uniformity.     

迭代目标因子分析-紫外分光光度法测定克感敏片三组分

本文应用迭代目标因子分析－紫外分光光度法不经分离同时测定克感敏 片中非那西丁、氨基比林、咖啡因三组分含量,其回收率和相对标准偏差分别为100．4％,0．83％,99．2％,0．77％,99．4％,0．69％。     

Development of a green effervescence-assisted dispersive liquid–liquid microextraction method using a home-made tablet disperser for trace analysis of Cd(II) and Pb(II)

An analytical approach for the determination of trace amounts of Cd(II) and Pb(II) has been developed using a home-made tablet-based effervescence-assisted dispersive liquid–liquid microextraction (DLLME) method which was performed in a narrow-bore tube, followed by flame atomic absorption spectrometry. In this method, a mixture of tartaric acid, sodium bicarbonate and NaCl was used to make the disperser tablet. Then, microlitre level of an extraction solvent was added in the tablet, and then, it was released into a narrow-bore tube containing sample solution and a complexing agent. An acid–base reaction immediately occurred between tartaric acid and sodium bicarbonate, and the produced CO₂ led to the dispersion of the extraction solvent into the solution as tiny droplets and subsequent extraction of the analytes. The method made possible the determination of Cd(II) and Pb(II) in the ranges of 0.1–10 and 1.0–20 µg L^?1, respectively. The limits of detection were obtained 0.43 and 0.05 µg L^?1 for Pb(II) and Cd(II), respectively. The limits of quantifications were 0.80 and 0.09 µg L^?1 for Pb(II) and Cd(II), respectively. Repeatability of the method, which is expressed as relative standard deviation, was obtained 3.1% (n = 6, C = 2 µg L^?1) and 1.3% (n = 6, C = 0.2 µg L^?1) for Pb(II) and Cd(II), respectively. The accuracy of the developed method was verified by analysing a certified reference material, namely SPS-WW2 Batch 108. Relative recoveries (84–107%, obtained at three fortification levels) confirmed the usefulness of the method for analysis of the analytes in the environmental water samples and fruit juices. The method was shown to be fast, reliable and environmentally friendly with low organic solvent consumption.     

Development of a sustained-release matrix tablet formulation of DHEA as ternary complex with α-cyclodextrin and glycine

Sustained-release matrix-tablets of dehydroepiandrosterone (DHEA) as ternary complex with α-cyclodextrin and glycine (c-DHEA) were prepared by direct compression with suitable excipients. The influence of the swelling properties of hydroxypropylmethylcellulose (HPMC) and the disintegrating power of Explotab^® used in combination, as well as the effect of the presence, type and amount of suitable channelling agents (Emcocel^® and spray-dried lactose, alone or in combination) on drug release behaviour from matrix-tablets has been evaluated. The best performances in terms of drug release was obtained from formulations containing a 75:25 w/w spray-dried lactose:Emcocel^® combination in the presence of HPMC as matrix-forming polymer, leading to a more than 65% DHEA released at the end of the test, a value which was, respectively, 1.9 and 2.7 times higher than those achieved with the corresponding formulations containing spray-dried lactose or Emcocel^® alone. The drug release profile from the most effective matrix-tablet formulation of c-DHEA allowed achievement of a more than 6-fold increase in the drug amount released within 24 h in comparison with the same formulation containing the simple physical mixtures of DHEA, α-cyclodextrin and glycine. Therefore the advantage of using DHEA as ternary complex, prepared by mechano-chemical treatment, was clearly demonstrated, thus allowing the development of an effective sustained-release formulation of the drug.     

A solid-phase enzyme-linked assay for vitamin B12

A new solid-phase enzyme-linked competitive binding assay for vitamin B₁₂ (cyanocobalamin) is described. The assay is based on the competition between analyte B₁₂ molecules and a glucose-6-phosphate dehydrogenase-vitamin B₁₂ conjugate for a limited number of R-protein binding sites immobilized on sepharose particles. After appropriate incubation and washing steps, the enzyme activity bound to the solid-phase is inversely related to the concentration of B₁₂ in the sample. Under optimized conditions, the method can detect B₁₂ in the range of 3×10^–10–1×10^–8 M (using 100l sample) with high selectivity over other biological molecules.