微流控芯片非接触电导法测定药品中的精氨酸布洛芬含量

建立了微流控芯片非接触电导检测快速测定精氨酸布洛芬含量的方法。考察了缓冲液种类和浓度、添加剂、分离电压以及进样时间等因素对分离检测的影响。优化条件为:20 mmol/L Tris-20 mmol/L H3BO3(p H 8.6)为缓冲溶液、不加添加剂、分离电压2.0 k V、进样时间10.0 s,在45.0 s内可实现精氨酸布洛芬的快速分离测定。结果表明,布洛芬和精氨酸在80.0~1.00×103mg/L范围内线性关系良好,相关系数(r)分别为0.998和0.997,检出限(S/N=3)为60 mg/L,相对标准偏差分别为1.9%和1.8%,加标回收率分别为97.9%~103%和97.3%~102%。该方法快速、简便,为精氨酸布洛芬非甾体抗炎药物的分析和质量控制提供了一种新方法。     

微乳体系相图及其在液相色谱分离多组分药物应用的研究

采用滴加法和电导率法绘制了十二烷基硫酸钠(SDS)/正丁醇/油相(正辛醇、正辛烷、正庚烷、正己烷)/水四组分微乳体系的拟三元相图。以O/W型微乳区域大小为指标,考察不同油相、表面活性剂与助表面活性剂的质量比对微乳形成的影响,并通过测定电导率、相对粘度以及表面张力等物理化学参数,考察了微乳体系的相行为及特性。根据得到的微乳体系相图,进行色谱条件优化,建立了快速、稳定的测定阿莫西林舒巴坦匹酯片剂中阿莫西林与舒巴坦匹酯二组分含量的方法,结果显示此微乳分离系统有较好的色谱适用性及方法可行性。     

Fast Determination of Ethylendiamine in Aminophylline Tablets by Small-sized Capillary Electrophoresis with Amperometric Detection

A novel method for fast determination of ethylendiamine (EDA) in Aminophylline Tablets has been developed by small‐sized capillary electrophoresis with amperometric detection (small‐CE‐AD) coupled with field‐amplified sample injection (FASI). Under the optimum conditions, EDA and four aliphatic diamine homologs (1,3‐diaminopropane, 1,4‐diaminobutane, 1,5‐diaminopentane and 1,6‐diaminohexane) could be well separated within 6 min at a separation voltage of 2.0 kV in an acetate buffer solution of pH 3.8 with low limit of detection (LOD) of 1.3×10^?11 g/mL for EDA (S/N=3). The proposed method has been successfully applied to direct determination of EDA content in different batches of Aminophylline Tablets. The method does not require off‐line preconcentration and derivatization steps, which should find wide application fields including pharmaceuticals as an alternative to conventional and microchip CE approaches.     

格列吡嗪片血药浓度的灰色药物动力学模型

应用灰色理论研究格列吡嗪片剂在健康志愿者体内的药物动力学模型. 8名健康志愿者口服格列吡嗪片5 mg后,用HPLC法测定不同时间血清中血药浓度,并建立格列吡嗪片在体内的灰色药物力学模型.预测值与实测值的平均绝对误差E =0 .5 3 2 ,平均相对误差为1 .0 5 9% ;达峰时间tmax =2 .5 6h;达峰浓度Cmax=0 .3 85 8μg/ml;曲线下总面积AUC =2 .75 44(μg/ml) * hour.该灰色模型的建立为格列吡嗪片剂的临床合理化用药提供了理论依据.     

复方甲硝唑片含量测定方法的比较

文章经选择适当的测定波长,同时采用系数倍率法和联立方程组新解法不经提取分离直接测定复方甲硝唑片中甲硝唑和维生素B_6的含量。同时采用河北省药品标准法进行了对比测定。利用SPSS统计软件通过对各方法的测定结果做方差分析,结果表明:新建立的系数倍率法和联立方程组新解法的测定结果无显著性差异,而两法分别与河北省药品标准法的测定结果比较,均存在显著性差异。作者认为:河北省药品标准法经过烦琐的提取分离过程,引入的误差较大。而新建立的两法简便、快速、准确,优于河北省药品标准法。     

Calibration in non-linear NIR spectroscopy using principal component artificial neural networks

Near-infrared (NIR) spectroscopy was used in simultaneous, non-destructive analysis of antipyriine and caffeine citrate tablets. Principal component artificial neural networks (PC-ANNs) were used to construct models for the analytes, using the testing set for external validation. Four pretreated spectra, namely, first-derivative, second-derivative, standard normal variate (SNV) and multiplicative scatter correction (MSC) spectra led to simplified and more robust models than conventional spectra. In PC-ANNs models, the spectra data were analyzed by principal component analysis (PCA) firstly. Then the scores of the principal compounds (PCs) were chosen as input nodes for input layer instead of the spectra data. The artificial neural networks (ANNs) models using the spectra data as input nodes were also established, which were compared with the PC-ANNs models. The result shows the SNV model of PC-ANNs multivariate calibration has the lowest training error and predicting error. The concept of the degree of approximation was introduced and performed as the selective criterion of the optimum network parameters.     

Rapid quantitative analysis of adulterant Lonicera species in preparations of Lonicerae Japonicae Flos

Lonicerae Japonicae Flos is often adulterated with Lonicerae Flos, which is derived from the other four Lonicera species, in both the crude drug and Lonicerae Japonicae Flos preparations. We proposed a methodology for the quantitative analysis of adulterant Lonicerae Flos in Lonicerae Japonicae Flos preparations. Taking macranthoidins A, B, dipsacoside B (saponins), sweroside (iridoids), and luteolin‐7‐O‐d ‐glucoside (flavonoids) as markers, a method of ultra high performance liquid chromatography with triple quadrupole mass spectrometry was employed to determine their amounts in Lonicerae Flos, Lonicerae Japonicae Flos, and Lonicerae Japonicae Flos preparations. The proportion of adulterant Lonicerae Flos in Lonicerae Japonicae Flos preparations was estimated based on the saponin contents of Lonicerae Japonicae Flos and Lonicerae Flos. All analytes separated under isocratic elution in 12 min with acceptable linearity, precision, repeatability, and accuracy. Lonicerae Japonicae Flos was easily distinguished from Lonicerae Flos by the total amount of saponins (0.067 and > 45.8 mg/g for Lonicerae Japonicae Flos and Lonicerae Flos, respectively). Eighteen of twenty one Lonicerae Japonicae Flos preparation samples were adulterated with Lonicerae Flos in proportions of 11.3–100%. The developed ultra high performance liquid chromatography with triple quadrupole mass spectrometry method could be used for the identification of Lonicerae Japonicae Flos and the four species of Lonicerae Flos and for the analysis of Lonicerae Japonicae Flos preparations adulterated with Lonicerae Flos.     

高效液相色谱法同时测定诺诺感冒片中扑尔敏、扑热息痛、盐酸伪麻黄碱的含量

 采用反相高效液相色谱法 ,在C18柱上以V(甲醇 )∶V(水 ) =2 5∶75的溶液为流动相 (内含 0 .0 5mol/L磷酸二氢钠 ) ,检测波长为 2 0 5nm ,同时分离测定诺诺感冒片中扑尔敏、扑热息痛、盐酸伪麻黄碱的含量。扑尔敏、扑热息痛和盐酸伪麻黄碱的检出限分别为 1.16mg/L ,0 .15mg/L和 1.82mg/L ,其相应的回收率分别为 98.35 % (n =5 ,RSD =1.6 0 % ) ,10 1.16 % (n =5 ,RSD =1.5 0 % )和 98.5 0 % (n =5 ,RSD =1.5 9% )。方法简便、快速 ,重现性好 ,适用于诺诺感冒片的质量检验分析。     

共轭梯度分光光度法用于克感敏片的含量测定

本文分析探讨了最优化方法中共轭梯度法用于处理多组分复方制剂的分光数据，给出了实际应用的迭代计算程序。通过克感敏片的模拟分析结果表明，各组分的平均回收率均在９９％～１０１％范围之内，变异系数（ＣＶ％）均小于２．５％。样品测定结果与标准方法基本一致。     

Simultaneous Determination of Ibuprofen and Pseudoephedrine Hydrochloride in Pharmaceutical Tablets by Reversed-Phase HPLC

Abstract

An isocratic HPLC method was developed and validated for the simultaneous determination of ibuprofen (IBU) and pseudoephedrine hydrochloride (PSE). Chromatography was carried out on an Apex phenyl column using 0.025 M acetic acid, triethylamine solution (pH 4.5) – acetonitrile (80:20, v/v) as mobile phase at a flow rate of 1 mL · min^?1. UV detection was performed at a wavelength of 210 nm. The method was validated for specificity, linearity, accuracy, precision, and was successfully applied to pharmaceutical tablets of Rhinadvil®.