Determination of vanadium in food and traditional Chinese medicine by graphite furnace atomic absorption spectroscopy

Various experimental conditions were described for the vanadium determinationby graphite furnace atomic absorption spectroscopy (GFAAS). The experiments showed that whenatomization took place under the conditions where the combination of a pyrolytic coating graphitetube and fast raising temperature were used and the temperature was stable, the signal peak shapescould be improved, the sensitivity was enhanced, and the memory effect was removed. The vanadium infood and traditional Chinese medicinal herbs can be accurately determined using the standard curvemethod.

A Novel Sample Introduction Technique for the Simultaneous Determination of As,Se,Ge and Hg in Chinese Medicinal Material

A novel technique of Moveable Reduction Bed Hydride Generator（MRBHG）was applied tohe hydride generation or cold vapor generation of As，Se，Ge，and Hg existing In TraditionalChinese Medicinal Material（TCM）．The simultaneous determination of the multi－elements wasperformed with ICP－MS．A solid reduction system involving the use of potassiumtetraborohydride and tartaric acid was applied to generating metal hydride or cold vaporefficiently．The factors affecting the metal cold vapor generation were studied．The mainadvantage of the technique is that only a 4μL volume of sample was required for the cold vapor

Research of Quality Standards for Stachydrine Hydrochloride in Chinese Medicine TJF Granule

A high-performance liquid chromatographic method was applied to the determination of stachydrine hydrochloride concentration in TJF granule (Chinese name: Tiao-Jing-Fang), using a mobile phase of methanol-acetonitrile (50:50, v/v) by the Agilent Kromasi NH2 column (250 mm × 4.6 mm, 5 μm, S/N: 22N25110). Detection wavelength was 201 nm. The result revealed good linearity of stachydrine hydrochloride and was obtained within the range of 0.20 - 1.98 μg/mL (R = 0.9995). The average recovery was 97.01%;the relative standard deviation (RSD) was 0.19%. To the best of our knowledge, this is the first report dedicated to the determination of stachydrine hydrochloride by the evaporative light scattering detector-high-performance liquid chromatographic (ELSD-HPLC) method.

Development and Validation of an HPLC Method for Simultaneous Determination of Nine Active Components in ‘Da-Chai-Hu-Tang’

In this study, a simple, reliable and accurate method for the simultaneous separation and determination of naringin, hesperidin, neohesperidin, baicalin, wogonoside, baicalein, wogonin, emodin and chrysophanol in ‘Da-Chai-Hu-Tang’ was developed by reverse-phase high-performance liquid chromatography (RP-HPLC). The chromatographic separation was performed on an Agilent ZORBAX C18 column (250 mm × 4.6 mm i.d., 5.0 μm), and the mobile phase composed of methanol and water containing 1% (v/v) acetic acid was used to elute the targets in a gradient elution mode. The flow rate and detection wavelength were set at 0.8 ml/min and 280 nm, respectively. All calibration curves of the nine components expressed good linearities (r2≥0.9992) within the tested ranges. The RSD values demonstrated the intra- and inter-day precisions were less than 2.89%, and the recoveries of the investigated compounds were between 96.22% and 105.28%. The proposed method is simple, precise, specific, sensitive, and successfully applied to determine the nine marker compounds in ‘Da-Chai-Hu-Tang’ for quality control.

A SERIES OF STRATEGIES FOR SOLVING THE SHORTAGE OF REFERENCE STANDARDS FOR MULTI-COMPONENTS DETERMINATION OF TRADITIONAL CHINESE MEDICINE

The shortage of reference standards has become the bottleneck of quality control of TCMs.In this study,a series of strategies,including one single reference standard to determine multi-compounds(SSDMC),quantitative analysis by standardized reference extract(QASRE),and quantitative nuclear magnetic resonance

NOVEL APPROACHES FOR THE DETERMINATION OF MULTIPLE PARTICULAR PESTICIDES IN TRADITIONAL CHINESE MEDICINES WITH COMPLEX MATRICES

The pesticide contamination of Traditional Chinese Medicines(TCMs)takes different ways,which caused the complexity of pesticide residues.The effective control of pesticide residues and the establishment of relevant detection methods are very important for ensuring the safety of TCMs.Our group has been committed to the determination of pesticide residues in TCMs for years.

Determination of strychnine and brucine in traditional Chinese medicine preparations by capillary zone electrophoresis with micelle to solvent stacking

A novel micelle to solvent stacking on-line sample preconcentration technique in capillary zone electrophoresis（MSS-CZE） has been developed to determine the strychnine and brucine in traditional Chinese medicine preparations.The optimal running buffer was 30 mmol/L H_3PO_4 containing 20%acetonitrile at pH 4.0.The sample matrix was 8 mmol/L H_3PO_4 containing 5 mmol/L sodium dodecyl sulfate（SDS） at pH 3.0.The established MSS-CZE method afforded more than 50-fold improvements in concentration sensitivity compared with typical CZE-UV analysis.The calibration curve was linear in the range from 0.2 to 15.0μg/ mL for both strychnine and brucine,with correlation coefficients of 0.9984 and 0.9976,respectively.The limits of detection（5/ N = 3：1） for strychnine and brucine were 0.02 and 0.05μg/mL,respectively.The MSS-CZE method has been successfully applied to the analysis of strychnine and brucine in Chinese medicinal preparations.

基于SCORE-TCM的中医药团体标准抽样评价方案设计

目前,各社会团体积极参与中医药标准的制定和发布,特别是“十四五”以来,中医药团体标准化工作更是迎来了提质增效的关键阶段。深入评估社会团体发布的中医药标准质量,是推进中医药团体标准工作的关键环节和重点任务。前期已研制并形成了中医药团体标准评价体系(System of Consortium Standards Rating and Evaluation of Traditional Chinese Medicine, SCORETCM)。在上述背景下,本研究通过专家共识法,设计了一套基于SCORE-TCM的中医药团体标准抽样评价方案,应用场景为对于特定社会团体发布的标准,或各团体发布的特定技术类别的标准进行快速评估。该方案涵盖了标准抽样、材料收集、标准评价、结果解读的完整流程,为中医药团体标准的抽样评价工作提供了参考方案。

融合Lasso的近似马尔科夫毯特征选择方法

在特征选择问题中,近似马尔科夫毯常用于判断冗余特征,但所得到的冗余特征并不完全相同,因此,在直接使用近似马尔科夫毯删除冗余特征时,存在可能导致信息丢失的情况,影响模型精度。为此,提出一种用于中药代谢组学高维小样本数据的融合Lasso的近似马尔科夫毯特征选择方法。方法分为两个阶段,第一阶段,通过最大信息系数对特征的相关度分析过滤无关特征;第二阶段,采用近似马尔科夫毯构建相似特征组,使用Lasso评估相似特征组中特征影响力,迭代去除冗余特征。通过实验对比表明,该算法可以在一定程度上减少有用信息丢失,去除无关特征和冗余特征,提高模型精度和稳定性。

液相微萃取技术应用于中药分析的研究进展

中药成分复杂,对样品进行前处理时常采用传统的提取方式,使用到大量的有机试剂,污染实验环境,影响人员健康,且实验废液的处理耗费大量的人力物力和财力。液相微萃取技术操作快速高效,使用试剂环境友好,成本低,此技术成为近年来研究的热点。通过查阅文献,从液相微萃取模式和液相微萃取溶剂两个方面对液相微萃取技术发展进行研究,展望了液相微萃取技术在中药分析方向的应用前景。

定量核磁共振技术在中药质量控制中的应用进展

中药质量控制是保证中药安全有效、质量稳定的基础,是中药标准化、现代化、国际化的前提,选用合适的分析方法在中药质量控制中具有重要意义。与薄层色谱、气相色谱、高效液相色谱等常规分析方法相比,定量核磁共振技术(qNMR)样品前处理简单、分析检测速度快、无需自身对照品,集定性鉴别和定量分析于一体,适用于中药中各类成分的检测分析,或将作为一种有力的分析技术,应用于中药质量控制。对qNMR的基本原理、定量方法和药典应用进行总结,重点介绍了qNMR在中药材、中药制剂、中药对照品及中药生产过程质量控制中的应用进展,提出了qNMR存在的若干问题并展望了其发展前景,旨在为采用qNMR控制中药质量提供参考。

HPLC法测定中药热敷包中羟基红花黄色素A的含量

目的建立中药热敷包中羟基红花黄色素A的含量测定方法。方法采用Agilent 1260高效液相色谱仪测定热敷包中羟基红花黄色素A的含量,样品用25%乙醇超声提取40 min。Kromasil C18色谱柱(4.6 mm×250 mm,5μm),柱温:30℃;流动相为乙腈-甲醇-0.7%磷酸水溶液(2∶26∶72),流速:1.0 ml·min^(-1);检测波长:403 nm。结果羟基红花黄色素A在0.511~1.789μg范围内与其色谱峰面积有良好的线性关系(r=0.9999),该方法的平均回收率为98.65%,RSD为0.61%(n=6),3批中药热敷包中羟基红花黄色素A平均含量为0.83 mg·g^(-1)。结论本法稳定可靠,重复性好,可用于中药热敷包的质量检测。

中药含量测定不同方法的比较

药品质量和安全直接关系到人民群众的健康和安全,文章对中药含量测定进行了全面概述,包括其背景、意义、基本原则与要求,并分析了传统含量测定方法和现代仪器分析方法的特点,同时对这些方法进行了比较与评价。通过引入具体实例,阐述了各种方法在实践测定上的运用情况,并对当前中药含量测定所面临的难点与挑战进行了分析探讨。最后,对中药含量测定技术面临的问题提出几点建议,为中药研究和发展提供了有力的技术和支撑。

Magnetic nanoparticles used in headspace extraction coupled with DSI-GC-IT/MS for analysis of VOCs in dry Traditional Chinese Medicine

A novel magnetic method using polystyrene modified magnetic nanoparticles to perform thermoheadspace extraction was successfully developed for extraction and preconcentration of volatile organic components in dry Traditional Chinese Medicine（TCM） based on gas chromatography-ion trap/mass spectrometry with a Chromato Probe direct sample introduction device. The dried fruit of Amomum testaceum Ridl. was used as the object TCM. The optimum parameters of headspace magnetic solid-phase extraction were investigated, in which desorption solvent ethyl acetate played a key role in this method,and the headspace extraction temperature of 90℃ and the headspace extraction time of 15 min finally decided. Headspace solid-phase microextraction method was also used to analyze volatile compounds in the TCM to compare with the proposed method. The results show that 60 components were identified totally by two methods; most of the low boiling point chemical compounds are isolated by this new method. In this work, an environmental-friendly and cheap analytical method was established, and a new approach to analyze volatile compounds in dry Traditional Chinese Medicine was also provided.

中药气味的化学成分检测及物质基础研究进展

气味是中药的重要感官指标,与中药品质及药效作用直接相关。一些常用中药具有特殊的气味,也是其鉴别和品质评价的重要指标。从化学物质基础角度来说,挥发性化学成分的种类和含量差异,导致了不同中药气味的异同。研究中药气味的化学物质基础对中药的综合质量控制、临床应用辅助、科学内涵解释等中药现代研究具有重大意义,而目前阶段对中药气味的研究,主要集中在挥发油的成分、制剂工艺和药理作用方面,以及使用感官分析设备对中药气味进行现代表征和区分,而对中药气味的分类和化学物质基础尚未有较为系统的总结和介绍。本文从中药气味检测技术、气味的感官分类、气味的化学物质基础和中药制剂生产过程中气味的变化规律等方面对此主题进行综述,并对其研究方向进行展望。

斜率校正一测多评法同时测定茯苓中3种三萜酸成分的含量

目的建立新的一测多评法同时测定茯苓中3-O-乙酰基-16α-羟基-氢化松苓酸、去氢茯苓酸和茯苓酸的含量。方法以Agilent ZORBAX SB-C_(18)(4.6 mm×250 mm,5µm)为色谱柱,以乙腈-0.1%磷酸水溶液为流动相等度洗脱;流速:0.8 mL/min;进样量:10µL;柱温:30℃;检测波长为210 nm。以茯苓酸为内参计算其他两个成分的校正因子。结果以茯苓酸为内参,3-O-乙酰基-16α-羟基-氢化松苓酸和去氢茯苓酸的校正因子分别为0.71和1.43;一测多评法测定结果与外标法测定结果无明显差异[相对误差(RE)<5%]。结论建立的一测多评方法简便准确,可用于茯苓药材中多指标成分的含量测定,为茯苓药材质量评价提供参考。

石榴皮菝葜复方搽剂指纹图谱的建立及3种成分的含量测定

目的建立石榴皮菝葜复方搽剂(SLPBQ)指纹图谱,结合化学模式识别方法进行分析,并对主要成分进行含量测定。方法采用Waters XBriage C18色谱柱(4.6 mm×250 mm,5μm),流动相为乙腈(A)-水(B),梯度洗脱,流速1.0 mL·min^(-1),进样体积10μL,检测波长270 nm,柱温30℃。采用《中药指纹图谱相似度评价系统(2012版)》绘制10批次SLPBQ的HPLC指纹图谱,确认共有峰,并分析多批次复方搽剂相似度。利用SPSS22.0及SIMCA-P14.1数据分析软件进行化学模式识别分析。通过单味药材及阴性对照图谱结合对照品比对指认化学成分,并对部分主要成分进行定量分析。结果10批次样品筛选出22个共有峰,且相似度均大于0.974;聚类分析将10批样品分为两大类;主成分分析筛选出5个主成分,累计方差贡献率为98.79%。对3种成分进行定量检测,发现各成分在各自浓度范围内的与峰面积线性关系良好(r≥0.9999),加样回收率为95.87%~103.76%,RSD均≤2%。结论该方法可用于SLPBQ的质量控制,简便、重复性好、稳定性好、准确度高。

子午流注针法联合中药熏蒸治疗水样液缺乏性干眼症疗效研究

目的:探讨子午流注针法联合中药熏蒸治疗水样液缺乏性干眼症的疗效及对患者泪膜稳定性的影响。方法:依据随机数字表法分配原则将110例水样液缺乏性干眼症患者分为对照组(55例)和治疗组(55例)。对照组给予聚乙二醇滴眼液进行治疗,治疗组在对照组基础上给予子午流注针法联合中药熏蒸进行治疗,两组均持续治疗6周。比较两组治疗6周后的临床疗效,对比两组治疗前及治疗6周后的症状积分、泪膜稳定性、细胞因子、视觉相关生命质量及治疗期间的安全性。结果:治疗组治疗6周后的总有效率为94.55%,高于对照组的78.18%(P<0.05)。治疗6周后,两组眼干涩、异物感、视疲劳、畏光、眼红、眼胀痛、泪液分泌量(SIT)、泪膜破裂时间(BUT)、角膜荧光素染色(FL)评分及血清基质金属蛋白酶-9(MMP-9)、白细胞介素-1β(IL-1β)、泪液白细胞介素-6(IL-6)、肿瘤坏死因子-α(TNF-α)、超敏C反应蛋白(hs-CRP)水平与治疗前比较均降低,治疗组低于对照组(P<0.05);两组视力障碍、活动障碍、一般健康状况评分与治疗前比较均升高,治疗组高于对照组(P<0.05)。两组治疗期间均未出现腹泻、眼部刺激、过敏等情况。结论:子午流注针法联合中药熏蒸可明显调节水样液缺乏性干眼症患者血清细胞因子水平,缓解机体炎症,提高泪膜稳定性,改善临床症状,进而可促进患者视觉相关生命质量的提高,疗效显著,安全性良好。

黄芩苷的药理活性及其定性定量分析检测方法的研究进展

黄芩苷是一种天然存在的黄酮类化合物,是从双子叶唇形科植物黄芩的干燥根中提取分离的,具有抑菌、抗炎、抗血栓、泻火解毒、止血安胎、抗变态反应、改善代谢异常和肠道菌群、修复肺损伤、抗辐射作用等多种药理活性。因此,研究中药有效成分的定性与定量分析方法具有重要意义。概述了黄芩苷的物化性质及药理活性,综述了近年来中药多组分中黄芩苷的定性与定量分析方法,以期为黄芩苷的检测技术及相关药物质量控制提供参考。

刍议《中华人民共和国药典》中药材项下的含量测定

通过对1953年版至2020年版《中华人民共和国药典》中中药材项下的含量测定的指标成分数量进行分析,统计中药含量测定在建国以来的历版药典的变化趋势,结果为:《中华人民共和国药典》收载的含量检测项下一个指标的中药材所占比例越来越高,两个指标的中药材从1990年版开始所占比例也是越来越高。随着科学技术的广泛运用,中药中被发现的化学成分越来越多,出现多个指标的含量检测的中药数量将会越来越多。中药质量的控制,我们肯定以代表成分作为其质量控制在一定范围内的积极作用,也要考虑在中医药理论指导下,综合权衡中药基原、种植/养殖、采收、加工、炮制、剂型、临床配伍和使用以及其不同药用部位都可影响到中药临床的安全性和有效性。在中药传承创新发展过程中,需做到充分尊重中医药理论体系的指导,以切合中医药特色的中医药思维对中药质量进行控制和管理,建立符合中药特点的质量管理标准,发挥中医药的特色和优势。