基于高效液相色谱-四极杆飞行时间串联质谱法的苦杏仁与桃仁化学成分差异研究

采用高效液相色谱-四极杆飞行时间串联质谱(HPLC-Q-TOF MS)技术对苦杏仁与桃仁甲醇提取物中的化学成分进行鉴定,同时利用化学模式识别方法分析了2种中药的差异成分。采用Agilent SB-C18(150 mm×3.0 mm,2.7 μm)色谱柱分离,以乙腈-0.1%甲酸水溶液为流动相进行梯度洗脱,质谱采用电喷雾离子源,在正、负离子模式下采集数据。对色谱图中各色谱峰进行精确质量数识别,结合数据库及二级质谱裂解规律对化学成分进行定性分析。利用 Profinder软件进行预处理,结合 SIMCA-P软件,建立了主成分分析(PCA)与正交偏最小二乘法判别分析(OPLS-DA)统计模型,进行差异性成分分析。苦杏仁与桃仁中共鉴定得到29个共有化学成分,其中苦杏仁苷、野黑樱苷、扁桃酸酰胺-β-龙胆二糖苷、扁桃酸-β-龙胆二糖苷、扁桃酸-β-D-吡喃葡萄糖苷和苄基-β-龙胆二糖苷等糖苷类化合物是苦杏仁与桃仁主要的难挥发化学成分。其中,15个化学成分在苦杏仁与桃仁中存在显著差异,主要包括糖苷类、氨基酸类与脂肪酸类等3类化合物。丙基-β-龙胆二糖苷在苦杏仁与桃仁中差异明显,可作为区分苦杏仁与桃仁潜在的化学标志物。该研究为苦杏仁与桃仁的药效研究及质量控制提供了数据支持。     

新工科背景下分析化学中质量保证和质量控制的教学改革探究*

通过对目前分析化学教学中存在问题的分析,探究了新工科背景下分析化学专业中关于质量保证和质量控制方面的教学改革,提出了增设“分析化学中的质量保证和质量控制”或者类似的课程的建议,指出分析化学的教学应该围绕整个分析过程展开,并将分析化学中的质量保证和质量控制知识融入分析全过程中,注重理论课程与实践课程相互结合的同时更加强调应用性,增强学生的实践能力和分析问题、解决问题的能力。此外,分析化学教学重在“分析”,要与分析实验室/检测机构保持紧密联系,应建立以市场为导向、以技术为核心的教学活动,从而实现为社会不断培养与时俱进的分析人才的教育目标。     

银莱汤中主要成分的UPLC多波长宽动态测定及质量评价研究

采用超高效液相色谱(UPLC)定量测定银莱汤中10种有效成分的含量并用于其质量评价.采用Wa-ters ACQUITY UPLC HSS T3色谱柱(2.1 mm × 100 mm,1.8 μm),以0.1％甲酸水溶液-0.1％甲酸乙腈为流动相梯度洗脱,3波长切换(0～10 min,320 nm;10～16 min,3...     

中药粉体物理指纹图谱研究进展

中药(TCM)粉体是中药口服固体制剂的重要中间体或产品,粉体的物理性质不仅影响制剂成型,而且直接或间接影响产品质量.中药粉体种类众多、尺度各异,采用物理指纹图谱可从物理状态层面整体评价中药粉体质量,并可将其作为对中药粉体含量测定或HPLC指纹图谱评价的补充,这为中药粉体全面质量控制提供了新的工具和思路.该文系统梳理了中...     

正负离子切换扫描质谱成像分析方法及其整体动物体内代谢应用研究

基于质谱成像(MSI)技术的空间分辨代谢组学方法已经成为生物组织学、肿瘤分子病理诊断和新药药效毒理研究的有力工具.该研究采用敞开式空气动力辅助解吸电喷雾离子化(AFADESI)技术,开发了一种正负离子切换扫描的质谱成像方法.该方法在离子化过程中无需施加高电压,既提高了敞开式离子化质谱成像的操作安全性,还可将生物组织切片...     

优质护理干预对帕金森患者心理情绪及生活质量的影响分析

目的分析优质护理干预对帕金森患者心理情绪及生活质量的影响。方法 70例帕金森病患者,随机分为干预组与对照组每组患者35例。对照组患者采用常规护理干预,干预组患者采用优质护理干预。结果两组SDS和SAS评分干预后较干预前降低,均有显著性意义(P0.05);干预组SDS评分和SAS评分干预后低于对照组,均有显著性意义(P0.05);两组ADL和MMSE评分干预后较干预前增加,均有显著性意义(P0.05);干预组ADL和MMSE评分干预后高于对照组,均有显著性意义(P0.05);两组物质生活、社会功能、心理健康和躯体功能评分干预后较干预前增加,均有显著性意义(P0.05);干预组物质生活、社会功能、心理健康和躯体功能评分干预后高于对照组,均有显著性意义(P0.05)。结论优质护理干预可减轻帕金森患者负性情绪,及提高患者生活质量。     

模块式护理计划对痛风患者疼痛及生活质量的影响分析

目的研究分析痛风患者采取模块式护理计划后对其生活质量、疼痛的影响。方法将佛山市第一人民医院风湿免疫内科2015年12月至2016年11月经临床诊断为痛风的住院患者156例随机分为常规组和实验组各78例,常规组采取常规护理措施,实验组采取模块式护理计划,比较两组患者的疼痛评分、疼痛缓解时间、生活质量评分。结果实验组、常规组疼痛缓解时间分别为(4.6±1.8)d、(7.3±2.7)d,(P0.05),护理2周后疼痛评分分别为(1.9±1.1)分、(4.1±2.5)分,(P0.05),生活质量评分分别为(8.2±2.6)分、(4.9±1.5)分,(P0.05)。结论模块式护理计划应用于痛风患者的护理中,能够显著降低患者的疼痛程度,提升其生活质量,缩短疼痛缓解时间,提高护理质量及效率,建议推广使用。     

Analytical Quality by Design (AQbD)-oriented RP-UFLC method for quantification of lansoprazole with superior method robustness

A reversed-phase ultrafast liquid chromatography method was developed for quantification of lansoprazole in pharmaceutical dosage form using analytical quality by design approach. Systematic planning and experimentation using design of experiment approach were used for method development and optimization studies. A central composite design was used for optimizing the chromatography, by choosing organic phase proportion and flow rate as the critical method variables for evaluating their effect on critical analytical attributes like resolution, plate number, and tailing factor. The optimal chromatography was accomplished on a C-18 column (250?×?4.6?mm, 5?µm) using methanol:water (70:30, v/v) as mobile phase at a flow rate of 1.0?mL/min. Photo diode array (PDA) detection was performed at 284?nm. Caffeine was used as the internal standard. Method validation studies revealed that the calibration curve was linear over 1.0–300?µg/mL. The method was found accurate with average recovery between 98.99 and 102.87%. The percent relative standard deviation values obtained for precision were as per ICH guideline and within the acceptance limits (<2%). Results of system suitability indicated superior method robustness. In a nutshell, the method was found to be highly suitable for its applicability in the determination of lansoprazole in bulk and tablet dosage form.     

Applications of Monte-Carlo simulation and chemometric techniques for development of bioanalytical liquid chromatography method for estimation of rosuvastatin calcium

In the present work, we investigated the development of a bioanalytical HPLC method of rosuvastatin (RSV) calcium as per the Quality by Design (QbD)-based systematic chemometric tools. At first, the method objectives were framed and critical analytical attributes (CAAs) were chosen. Risk assessment and factor screening was performed using Hybrid Risk Matrix and Plackett–Burman design for identifying vital factors influencing the critical method parameters (CMPs). Monte-Carlo simulation analysis was conducted which confirmed excellent process robustness (Ppk >1.33) for the studied ranges of CMPs. Furthermore, systematic method development was carried out using custom experimental design, where mobile phase ratio, pH, and injection volume were taken as CMPs at three levels. The obtained trials were evaluated for peak area, retention time, theoretical plates, and peak tailing as CAAs. Mathematical response surface modeling was carried out and optimal chromatographic solution was identified using response optimizer plots. Method transfer was made to bioanalytical scale for estimation of the analyte in rat plasma samples. Extensive method validation was performed as per the ICH Q2 guideline, which indicated validation parameters within the acceptable limits. Overall, the studies construed successful development of QbD compliant HPLC method of rosuvastatin with potential utility bioanalytical testing.     

加强助教培训和管理工作,提高化学实验教学质量

介绍了中国科学技术大学化学实验教学中心在实验助教培训和管理方面所开展的举措,从助教申请及培训流程、教学方法与技巧、考核制度、奖励措施等方面展开论述,分析了实验助教在本科实验教学中的作用,以及目前实验助教制度中存在的一些问题和解决方法。