非对称场流分离系统的构建及其在淀粉颗粒粒径表征中的应用

淀粉颗粒粒径与分子尺寸分别在1～100μm和20～250 nm之间,是影响淀粉功能特性的重要因素之一.非对称场流分离(AF4)是一种基于样品与外力场相互作用机制的分离技术,已应用于表征淀粉分子尺寸分布.商品化的AF4系统的粒径检测范围为1 nm～10μm,对于淀粉颗粒粒径表征具有一定的局限性.该文研制了AF4分离系统;...     

Analysis of chemical components in herbal formula Qi Bai Granule by UPLC-ESI-Q-TOF-MS

Qi Bai Granule (QBG), a traditional Chinese medicine formula for the treatment of idiopathic thrombocytopenic purpura, is composed of seven herbs. It is necessary to learn its chemical composition for quality control. In this study, a method for rapid separation and structural identification of the constituents in QBG was established by UPLC-ESI-Q-TOF-MS in negative and positive ion mode. As a result, 112 compounds, such as triterpenoids, flavonoids and monoterpenes were detected. Based on the retention times, accurate masses, fragment ions, related literatures, and/or authentic standards, 107 compounds were unambiguously identified or tentatively characterized. Additionally, 20% monarch, 50% minister, 5% assistant and 24% guide drugs of 112 compounds were detected, which on the whole was consistent with the compatibility of QBG. The results would provide a scientific basis for the quality control, quantitative analysis and further study in vivo or vitro of QBG.     

A sensitive UPLC–MS/MS method for simultaneous determination of polyphenols in rat plasma: Application to a pharmacokinetic study of dispensing granules and standard decoction of Cinnamomum cassia twigs

This study established a rapid and reliable approach using liquid chromatography–tandem mass spectrometry for the simultaneous determination of cinnamic acid, vanillic acid and protocatechuic acid in rat plasma. This is the first report on a comparative pharmacokinetic study of dispensing granules and standard decoction of Cinnamomum cassia twigs in rats. After liquid–liquid extraction by ethyl acetate, the plasma samples were subjected to LC–MS/MS for multiple reaction monitoring. The standard curves showed good linear regression (r² > 0.9991) in the range of 10.0–16000 ng/mL. The intra‐ and inter‐day accuracy and precision were found to be within 15% of the nominal concentration. The recoveries of the three phenolics ranged from 88.7 to 105.7%. Finally, this approach was successfully applied to pharmacokinetic analysis of the three phenolics after oral administration of standard decoction and dispensing granules of C. cassia twigs in rats. Although the values of AUC_0–t of vanillic acid and protocatechuic acid in standard decoction group were larger than those of the dispensing granule group, no significant difference was observed for the two groups. Of note, the elimination rates of vanillic acid were slower in the standard decoction group than the dispensing granule group.     

The metabolomic study on atherosclerosis mice and its application in a traditional Chinese medicine Sishen granule

Although an atherosclerosis (AS) model using low‐density lipoprotein receptor deletion mice has been widely applied, its pathological pathway in metabolite level is still not clear. To further reveal the metabolite profile and identify the potential biomarkers in AS development, a serum metabolomic approach was developed based on reversed‐phase liquid chromatography/quadrupole time‐of‐flight mass spectrometry (LC‐Q‐TOF‐MS). The established metabolomic platform was also used for elucidating the therapeutic mechanism of a traditional Chinese medicine named Sishen granule (SSKL). Twenty‐one potential biomarkers in AS mouse serum were identified. Through functional analysis of these biomarkers, inflammation, proliferation, dysfunction of energy metabolism and amino acid metabolism were considered the most relevant pathological changes in AS. DNA damage products were found for the first time in the metabolomic study of AS. The network established by 20 biomarkers revealed that pyruvate metabolism, citrate cycle, fatty acid metabolism and urea metabolism were seriously disturbed. This metabolomic study not only supplied a systematic view of the progression of AS but also provided a theoretical basis for the treatment of AS. This metabolomic study also demonstrated that SSKL had therapeutic effectiveness for AS through partly reversing the inflammation reaction and amino acid metabolism dysfunction. Copyright © 2015 John Wiley & Sons, Ltd.     

王老吉广东凉茶颗粒的超高效液相色谱指纹图谱研究

建立了适用于王老吉广东凉茶颗粒质量控制的超高效液相色谱指纹图谱分析方法。样品采用甲醇超声萃取30 min,萃取液用超高效液相色谱法进行指纹图谱分析。色谱柱采用Waters ACQUITY HSS T3 C18(3.0mm×150 mm,1.8μm),以0.5%甲酸-乙腈为流动相进行梯度洗脱,流速为0.8 mL/min,柱温35℃。28个共有峰在18 min内得到良好分离,通过对照品对其中4个峰进行了确证。对王老吉广东凉茶颗粒样品进行了相似度分析,23个批次样品的相似度均达到0.95以上;以28个共有峰的相对峰面积进行主成分分析,23批次样品均落在同一区域。相似度评价和主成分分析结果均表明,王老吉广东凉茶颗粒的产品质量稳定性好。该方法快速、高效、稳定,可用于王老吉广东凉茶颗粒的质量控制。     

HPLC-PDA法对中成药养心生脉颗粒中丹参素含量的测定

建立了用HPLC_PDA法测定养心生脉颗粒中丹参素含量的方法.采用Symmertry ShieldTMRP18(150 mm×4.6 mm,5μm)色谱柱;以V(甲醇)∶V(水)∶V(冰醋酸)=5∶94.5∶0.5为流动相;流速为1.0 mL/min;检测波长280 nm.丹参素在9.5~152 mg/L内,线性关系良好(R>0.999 9);加标回收率平均为98.9%,RSD为0.97%.为丹参类颗粒的质量综合评价和质量控制提供了简单、准确、可行的分析方法.     

颗粒系统竞争式聚集行为的计算机模拟

实现两种颗粒混合物的竞争式聚集行为的二维仿真模拟,编程时考虑颗粒与颗粒、颗粒与侧壁、颗粒与中央挡板以及颗粒与底板的碰撞.模拟结果表明:振动强度较小时,颗粒最终聚集到起初小颗粒多而大颗粒少的右室;振动强度较大时,颗粒最终聚集到起初大颗粒多而小颗粒少的左室;振动强度很大时,颗粒呈均匀分布状态,模拟与实验定性符合良好.     

聚羧酸系列分散剂在农药水分散粒剂(WDG)中的应用

采用清洁的水溶液聚合工艺,以丙烯酸、马来酸和功能单体为主要原料,分别以过硫酸盐、双氧水-金属盐体系、过马来酸体系等为引发剂合成了适宜结构的聚羧酸系列农药分散剂,考察和评价了其对水分散粒剂(WDG)的配伍性及稳定性,并进行了田间药效验证试验,结果表明,其性能达到国内外同类产品水平,具有较好的推广应用价值.     

二进制粒在旱涝序列相似性匹配中的应用

通过采用二进制数表示旱涝事件序列中的事件,描述了基于二进制信息粒的运算及二进制粒事件序列相似性匹配的相关定义,提出了基于二进制粒事件序列上的多层次全序列匹配算法及相关定义;经实验验证分析,说明了研究的有效性,为研究地域气候相似和局地小气候相似提供了新方法。     

甘草配方颗粒有机氯类农药残留量测定

目的：以气相色谱法对甘草配方颗粒剂中的9种有机氯农药残留量进行检测.方法：样品通过丙酮超声提取,经硫酸净化杂质,用DB-1701P弹性石英毛细管柱分离待测组分,ECD检测器进行检测.结果：9种有机氯农药线性回归方程的相关系数在0.9996～0.9999范围之内,线性关系良好,样品回收率为74.92％～1 15.0％,RSD为0.75％～7.89％.结论：本方法快速、简便、准确,能准确用于甘草配方颗粒中9种有机氯类农药残留的检测.