偏最小二乘法测定复方乙酰水杨酸片中的有效成分

将偏最小二乘法(PLS)与近红外漫反射光谱法相结合,对复方乙酰水杨酸片进行无损非破坏定量分析．建立了最佳的数学校正模型,比较了样品中3种有效成分(乙酰水杨酸、非那西丁和咖啡因)同时测定和单独测定时的主成分数对PLS定量预测能力的影响,预测了未知样品。3种有效成分同时测定和单独测定建立的PLS模型具有相同的主成分数,PLS预报浓度与参考浓度具有相近的标准偏差,说明用PLS法同时测定3种组分的含量是可行的。     

薄层色谱法测定复方乙酰水杨酸药片的含量

复方乙酰水杨酸药片(又称复方阿斯匹林,APC)是常用的解热镇痛药。其主要成分是阿斯匹林、非那西丁和咖啡因。对APC药片中这三种组分的分析一般采用容量法,此法操作繁琐,溶剂消耗量大。近来有文献报道采用光谱法测定咖     

吸光光度多组分同时测定方法研究——MR和PLS法测定钴、镍、铜三组分混合体系

用偏最小二乘法(PLS)和多元线性回归法(MR)分别对钴、镍、铜三组分混合体系进行同时测定,证明PLS法对光谱重叠严重的体系较MR法有更好的预报准确性.着重讨论了校正集样品数n、波长数,和特征变量数d等测定参数对预报结果的影响.     

多元校正-速差动力学分光光度法同时测定三组分有机磷农药

速差动力学分析结合化学计量学对动力学数据进行解析计算, 可扩大动力学分析的范围, 提高分析的准确度. 本文利用对硫磷、甲基对硫磷和杀螟硫磷在碱性介质中能与氧化剂过氧化氢发生氧化反应生成对硝基苯酚的性质, 引入多元校正方法中的经典最小二乘法(CLS)、偏最小二乘法(PLS)和主成分回归法(PCR)对动力学数据进行解析, 实现了三组分人工合成样品的同时测定.     

改进的迭代目标转换因子分析研究

本文用非线性迭代偏最小二乘法分解原始数据阵,提出了改进的迭代目标转换因子分析法,大大简化了运算,方法简单、直观、准确.用此法对复方扑热息痛片中三组分(乙酰基水杨酸、扑热息痛及咖啡因)的含量进行紫外光谱测定,结果满意.     

偏最小二乘法用于研究酚类物质的竞争吸附

将偏最小二乘法(PLS)用于紫外-可见分光光度分析,同时测定水溶液中苯酚、对甲氧基苯酚和α-萘酚三种组分,并将此方法用于研究苯酚、对甲氧基苯酚和α-萘酚在水溶液中的竞争吸附.结果表明:合成样本的回收率在96%~107.6%之间,结果比较令人满意.采用PLS法计算三种酚类物质吸附后的平衡浓度和吸附量,其结果与采用LCA(Langmuir Competitive Adsorption)模型预测的结果较为接近.     

主成分回归-紫外光度法同时测定食用香料麦芽酚和乙基麦芽酚

报道了一种快速、简便的同时测定食用香料麦芽酚、乙基麦芽酚光度法,方法基于在pH2.87的B R缓冲溶液中对麦芽酚和乙基麦芽酚两组分混合溶液进行光度测定,所得的重叠波谱数据用主成分回归法(PCR)、经典最小二乘法(CLS)和偏最小二乘法(PLS)等化学计量学方法进行处理,结果表明主成分回归法(PCR)的预报误差最小。对样品进行测定,获得了较好的定量分析结果。麦芽酚和乙基麦芽酚的线性范围均为1.0～20.0mg·L-1;检出限分别为0.4347和0 5589mg·L-1。     

蜂蜜中葡萄糖、果糖和木糖的多元校正定量分析研究

根据单糖与邻甲苯胺加成缩合反应的显色特征,采用偏最小二乘法(PLS)辅助分光光度法对吸收光谱重叠较严重、加和性欠佳的葡萄糖、果糖和木糖三组分的模拟混合试样进行分析,对同时测定的条件进行了优化,建立了单糖多组分体系同时定量分析的多元校正方法,并用此方法对蜂蜜样品中上述单糖组分的含量进行了测定.时模拟混合试样,回收率分别为...     

偏最小二乘法分光光度同时测定复方扑热息痛片中各组分含量

本文介绍了偏最小二乘法(PLS)用于多组分分光光度分析的基本原理和算法.研究了复方扑热患痛片中扑热息痛、阿司匹林和咖啡因的PLS测定方法,各组分的平均回收率分别为99.88±0.33％、99.99±0.14％和99.92±1.24％(置信度95％).     

主成分回归一紫外光度法同时测定盐酸西替利嗪和苯甲酸钠

提出了一种用紫外光度法同时测定盐酸西替利嗪和苯甲酸钠的方法.在pH 4.56的B-R缓冲溶液中对盐酸西替利嗪和苯甲酸钠两组分混合溶液进行吸光度测定,所得的重叠光谱数据用主成分回归法(PCR)和偏最小二乘法(PLS)等化学计量学方法进行处理,结果表明主成分回归(PCR)的预报误差最小.对实际样品进行测定,回收率为88.8...     

紫外多波长光谱法监测阿司匹林合成过程的水杨酸和阿司匹林

建立测定阿司匹林合成过程中水杨酸、阿司匹林含量和转化率的分析模型。采用紫外多波长扫描乙醇溶液中阿司匹林和水杨酸的紫外光谱,建立水杨酸和阿司匹林紫外光谱的向量长度与其质量浓度的标准曲线,通过斜投影算法分离出待测样本中阿司匹林和水杨酸的紫外光谱。计算光谱向量长度,代入标准曲线得到待测样本中阿司匹林和水杨酸的含量。实验结果表明,水杨酸、阿司匹林的质量浓度与其紫外光谱的向量长度呈良好的线性关系,线性范围分别为2.00~40.00,10.00~200.00μg/m L。水杨酸和阿司匹林测定结果的相对标准偏差为0.16%~2.19%(n=5),加标回收率在93.3%~106.9%之间。该方法快速简便、准确可靠,可满足阿司匹林和水杨酸的同时测定及反应过程中水杨酸转化率监测要求。     

基于子空间夹角判据监测阿司匹林合成体系中的水杨酸和阿司匹林

利用水杨酸、阿司匹林、乙酸酐和乙酸的多波长紫外光谱作为本底光谱库和样本光谱库,建立一种基于子空间夹角判据的快速定量分析阿司匹林合成体系中水杨酸和阿司匹林的方法。水杨酸、阿司匹林质量浓度范围分别在1.16～34.684,9.84～188.928μg/mL内,所测得水杨酸和阿司匹林检验集的R分别为0.999 7和0.999 1,RMSE分别为0.509 5,2.624 0μg/mL,效果优于普通波峰点最小二乘法和偏最小二乘法。水杨酸和阿司匹林的加标回收率在94.01%～106.44%之间,测定结果的相对标准偏差分别为3.45%和4.80%(n=7)。该方法可用于监测阿司匹林合成体系中的水杨酸和阿司匹林。     

高分子复合药物(阿司匹林和烟酸)的合成与表征

通过酰氯法分别由阿斯匹林和烟酸与甲基丙烯酸-2-羟基乙酯合成了含阿司匹林的可聚合单体(A)和含烟酸的可聚合单体(B)，然后将它们进行了聚合，得到了含阿司匹林和烟酸的复合药物。测定了A和B的竞聚率，产物经核磁共振及凝胶渗透色谱表征。     

Simultaneous determination of carisoprodol and aspirin in human plasma using liquid chromatography–tandem mass spectrometry in polarity switch mode: application to a human pharmacokinetic study

A simple, sensitive and rapid LC‐MS/MS‐ESI method has been developed and validated for simultaneous quantification of the carisoprodol and aspirin in human plasma. Carisoprodol was detected in positive ion mode, whereas aspirin was detected in negative ion mode. Carbamazepine and furosemide were used as internal standards (IS) for quantification of carisoprodol and aspirin, respectively. The extraction procedure involves a liquid–liquid extraction method with ter‐butyl methyl ether. Chromatographic separation was achieved on a Zorbax XDB‐Phenyl (4.6 × 75 mm, 3.5 µm) column using an isocratic mobile phase (5 mm ammonium acetate:methanol, 20:80, v/v) at a flow rate of 0.8 mL/min with a total run time of 2.2 min. A detailed method validation was performed as per the FDA guidelines. The standard curves found to be linear in the range of 25.5–4900 and 15.3–3000 ng/mL for carisoprodol and aspirin, respectively. The results met the acceptance criteria. Carisoprodol and aspirin were found to be stable in various stability studies. The validated method was successfully applied to a pharmacokinetic study following co‐administration of carisoprodol (250 mg) and aspirin (75 mg) tablets by oral route to human volunteers. Copyright © 2012 John Wiley & Sons, Ltd.     

Analgetic Activity of Papaya (Carica papaya L.) Leaves Extract

The analgetic activity of Carica papaya leaves (CPL) extracts (n-hexane, ethyl acetate, ethanol) was investigated in mice model using acetic acid induced pain (Siegmund method). Experimental animals were divided into 11 groups and received n-hexane, ethyl acetate, and ethanol extracts at doses of 0.175, 0.35, 0.70 mg/kg bw orally; CMC-Na 0.5% (control group); 50 mg/ kg bw of aspirin. The results showed that all extracts at the doses of 0.175, 0.35 and 0.70 mg/kg bw gave significant analgetic activity (p<0.05) compared to control group. Ethanol extract of CPL dose of 0.70 mg/kg bw showed the best analgetic activity that was comparable to aspirin.     

胶束电动毛细管色谱法同时测定阿咖酚散中3种有效成分

建立了胶束电动毛细管色谱同时分离测定阿咖酚散中咖啡因、对乙酰氨基酚、阿司匹林3种有效成分的方法。对以有机碱三乙醇胺为改进剂的胆酸胶束相进行了优化,对改进剂的影响机理进行了详细讨论。最佳电泳条件如下:以40 mmol/L硼酸盐-60 mmol/L胆酸-12.5%三乙醇胺(pH 12.0)为缓冲体系,分离电压为15 kV,检测波长为254 nm。在上述条件下,14 min内实现了阿咖酚散中3组分的基线分离。咖啡因、对乙酰氨基酚和阿司匹林的线性范围分别为18.75～900.0(r=0.999 9)、2.60～62.50(r=0.992 9)、79.17～3 800 mg/L(r=0.994 0)。上述3组分迁移时间和峰高的相对标准偏差分别不高于1.8%和6.8%。咖啡因、对乙酰氨基酚和阿司匹林的检出限分别为4.6、0.17、38 mg/L。应用该法测定阿咖酚散中上述3组分,加标回收率分别为100%、100%和102%,可满足实际样品分析要求。所建立的方法简便、快速、灵敏、经济,能同时进行阿咖酚散中多种成分的分离测定。     

高效液相法测定注射用赖氨匹林中的阿司匹林及游离水杨酸

 建立了高效液相法 (HPLC)同时测定注射用赖氨匹林中阿司匹林和游离水杨酸含量的方法。采用的柱为HypersilBDSC18柱 ,流动相为甲醇 水 冰醋酸 (体积比为 35∶6 5∶3) ,检测波长为 2 80nm。阿司匹林和水杨酸的质量浓度分别为 0 0 2 8g/L～ 0 14 1g/L和 0 77mg/L～ 3 85mg/L时线性关系良好 ,其线性相关系数分别为0 9999和 0 9998;加样回收率分别为 99 2 7% (RSD =0 8% )及 99 6 1% (RSD =1 3% )。     

Stability‐indicating HPLC method for simultaneous quantification of 14 impurities in excedrin tablet formulations and identification of new impurity by LC–MS in accelerated stability studies

We developed novel stability‐indicating HPLC method for simultaneous estimation of 14 impurities in excedrin tablet, a formulation with a combination of acetaminophen, aspirin, and caffeine. In addition, a new impurity that was generated through degradation of aspirin at high temperatures during the accelerated stability conditions was positively identified and confirmed, using liquid chromatography–mass spectrometry technique. The HPLC method was optimized using the Inertsustain C₁₈, 250 × 4.6 mm, 5.0 μm column, employing simple gradient method. Forced degradation studies were performed under acidic, basic, oxidative and thermal conditions to prove the scope and stability‐indicating the nature of the method. The optimized method was validated as per the International Conference on Harmonization guidelines. The HPLC method showed linearity from LOQ concentration to 21 μg mL^?1. Precision and intermediate precision values were <5% RSD. The validated HPLC method is currently applied for the routine testing of excedrin tablet formulations in quality control laboratories.     

Determination of acetylsalicylic acid and its major metabolite, salicylic acid, in human plasma using liquid chromatography-tandem mass spectrometry: application to pharmacokinetic study of Astrix in Korean healthy volunteers

The first liquid chromatography-tandem mass spectrometry (LC/MS/MS) method for determination of acetylsalicylic acid (aspirin, ASA) and one of its major metabolites, salicylic acid (SA), in human plasma using simvastatin as an internal standard has been developed and validated. For ASA analysis, a plasma sample containing potassium fluoride was extracted using a mixture of ethyl acetate and diethyl ether in the presence of 0.5% formic acid. SA, a major metabolite of ASA, was extracted from plasma using protein precipitation with acetonitrile. The compounds were separated on a reversed-phase column with an isocratic mobile phase consisting of acetonitrile and water containing 0.1% formic acid (8:2, v/v). The ion transitions recorded in multiple reaction monitoring mode were m/z 179 --> 137, 137 --> 93 and 435 --> 319 for ASA, SA and IS, respectively. The coefficient of variation of the assay precision was less than 9.3%, and the accuracy exceeded 86.5%. The lower limits of quantification for ASA and SA were 5 and 50 ng/mL, respectively. The developed assay method was successfully applied for the evaluation of pharmacokinetics of ASA and SA after single oral administration of Astrix (entero-coated pellet, 100 mg of aspirin) to 10 Korean healthy male volunteers.