Identification and quantitation of major phenolic compounds from penthorum chinense pursh. by HPLC with tandem mass spectrometry and HPLC with diode array detection

Penthorum chinense Pursh. is a traditional Chinese herbal medicine used for the treatment of various ailments specially related to liver. Gansu Granule, the medicine made from the extract of P. chinense, has been widely used in the clinical setting. But the information about its active ingredients is lacking. In this paper, the extract of P. chinense was analyzed by high performance liquid chromatography with electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry. Among the 27 compounds that were identified based on their mass spectrometry data, ten were reported for the first time from P. chinense. Chromatographic fingerprints generated by high‐performance liquid chromatography by analyzing 21 batches of P. chinense, displayed six common peaks. Finally, four major compounds were identified namely; gallic acid, brevifolin carboxylic acid, 2,6‐dihydroxyacetophenone‐4‐O‐β‐d‐ glucoside, and pinocembrin‐7‐O‐β‐d‐ glucoside. The average content of each compound was 24.58, 109.6, 15.52, and 18.81 mg/g, respectively. In addition, this study also suggests that the qualitative liquid chromatography with mass spectrometry and the quantitative high‐performance liquid chromatography analytical methods using monolithic columns are simple, rapid, accurate, and reproducible and have the potential to be used for the comprehensive quality control of P. chinense.     

Methods for the exploratory analysis of two-dimensional chromatographic signals

In this article several approaches for the exploratory analysis of two-dimensional chromatographic signals (fingerprints) are presented. Their usefulness is illustrated on experimental chromatographic data obtained from high performance liquid chromatography using the photodiode-array detector (HPLC-DAD). Among the methods discussed are principal component analysis (PCA), hierarchical clustering methods and several N-way techniques such as PARAFAC, PARAFAC2 and Tucker3. In addition to the N-way methods, other approaches that allow for comparing samples represented by two-dimensional fingerprints are also presented (the Rv coefficient, the STATIS approach and ‘fuzzy’ variants of the similarity matrix). Exploratory analysis of the HPLC-DAD data with peak shifts is also discussed.     

甘草参与的B-Z振荡反应研究

以H+-Mn2+-BrO-3-CH3COCH3-甘草组成的化学振荡体系,应用电化学工作站记录电位(E)随时间(t)的变化,绘制化学振荡曲线.通过考察反应条件及反应物的浓度等因素对振荡曲线的影响,优化最佳的振荡反应条件,计算反应的活化能,推断反应的机理.为利用此方法鉴别中草药及研究中药治疗疾病提供理论依据.     

蔬菜粉末荧光光谱测定及其在手印显现中的应用

对遗留在客体表面的手印进行提取和鉴定是侦破案件的重要依据。对在犯罪现场发现的手印进行固定提取时,首先应该使用没有破坏性的光学无损检验技术。实践表明光学无损检验技术对于绝大部分光滑客体上的手印都能取得很大的反差和较好的纹线细节,而对于光滑度较差的客体上的手印则需要使用有损的物理法和化学法对指印进行固定提取。其中粉末法和熏显法在手印显现中得到了广泛的应用,但是常用的绝大部分粉末和熏显物质对长期从事手印显现的工作人员身体有较大的毒副作用。而且绝大部分常用的荧光粉末需要在紫外线的激发下产生荧光,紫外线激发手印产生荧光的同时也常会激发承痕客体产生很强的背景荧光,进而降低了手印与背景的反差。因此寻找一种成本低廉、无毒无害、操作简单和应用性广泛的手印显现方法是当务之急。研究了三种无毒无害、成本低廉的蔬菜粉末的荧光性能,并且将其应用于手印显现中。首先通过荧光分光光度计测定西蓝花粉末、菠菜粉末和紫菜粉末的荧光激发光谱和荧光发射光谱。通过荧光测定发现,西蓝花粉末的荧光比菠菜粉末和紫菜粉末的荧光强很多,所以选择西蓝花粉末显现犯罪现场常见的疑难客体表面汗潜手印。实验结果表明：（1）西蓝花粉末、菠菜粉末和紫菜粉末都能发出荧光,荧光激发光谱峰值都在417 nm,荧光发射光谱峰值都在678 nm,其中西蓝花粉末发出的荧光最强。（2）将西蓝花粉末用于多色图案干扰的非渗透性和渗透性客体上的汗潜手印的显现中,在415 nm的紫光的照射下能够发出明亮的红色荧光。拍照荧光指印时在镜头前加上透过中心波长为680 nm左右的窄带通干涉滤光镜,结果显示手印纹线与背景反差强烈,纹线清晰连贯,消除背景的干扰。（3）与传统的荧光粉末显现法相比,该显现方法具有较高的显现灵敏度。（4）有些客体背景图案在415 nm的紫光的照射下也有发光,但与西蓝花粉末的非常强的荧光相比,背景的荧光弱得多,所以使得手印与背景之间形成了较大的反差并且纹线的细节特征清晰。（5）粗糙客体上手印的显现也获得了很大的反差,粗糙的背景没有对纹线形成干扰而形成了清晰连贯的纹线。（6）实验中使用的市售的西蓝花粉末具有颗粒细小、吸附能力强等特点,能够促进手印物质与西蓝花粉末之间的选择性吸附,进而进一步提高手印显现的灵敏度。     

血指印检测研究进展

犯罪现场血指印的发现和提取在案件侦破中起着非常重要的作用,是最有效的个人身份鉴定手段之一。血指印检测方法依据反应原理的不同分为化学方法、物理方法、生物染色和光学方法等4类。本文重点综述了血指印的检测技术、常用试剂及其优缺点,并展望了血指印检测方法的方向和前景。     

Differentiation of Cultivars of Flos Chrysanthemum with the Use of High-Performance Liquid Chromatography Fingerprints and Chemometrics

Flos Chrysanthemum is a generic name for a particular group of edible plants, which also have medicinal properties. There are, in fact, twenty to thirty different cultivars, which are commonly used in beverages and for medicinal purposes. In this work, four Flos Chrysanthemum cultivars, Hangju, Taiju, Gongju, and Boju, were collected and chromatographic fingerprints were used to distinguish and assess these cultivars for quality control purposes. Chromatography fingerprints contain chemical information but also often have baseline drifts and peak shifts, which complicate data processing, and adaptive iteratively reweighted, penalized least squares, and correlation optimized warping were applied to correct the fingerprint peaks. The adjusted data were submitted to unsupervised and supervised pattern recognition methods. Principal component analysis was used to qualitatively differentiate the Flos Chrysanthemum cultivars. Partial least squares, continuum power regression, and K-nearest neighbors were used to predict the unknown samples. Finally, the elliptic joint confidence region method was used to evaluate the prediction ability of these models. The partial least squares and continuum power regression methods were shown to best represent the experimental results.     

Multifarious Applications of Photoacoustic Spectrophotometer and Its Importance in Forensic Investigation

Abstract: Photoacoustic spectrophotometer (PAS) has emerged as the most promising technology with its promise to resolve unmet issues in various domains. The advantages of PAS are nonvulnerability of the sample, trace quantity sample analysis, and short response time. Though it showed distinguished features close to its emergence, it is bereft of its importance in the present scenario. Certainly, there exists a transparent gap in understanding the current situation in forensic crime scene management and the application of PAS within the same discipline. This article aims to consolidate all this information to fill an existing knowledge gap and tries to establish trajectory of research done up to now. This article will also pinpoint the reasons behind why this advanced technique could not accomplish its respectable feat inside the market and restraint of optical business toward inventing and commercializing this merchandise.     

金银花的13C NMR指纹图谱研究

利用PFT-NMR 核磁共振波谱仪测定了金银花特征提取物的¹³C NMR图谱,对金银花提取物的¹³C NMR指纹图谱进行了解析,与其有效成分绿原酸进行了比较,获得了金银花提取物的特征峰,并比较了不同金银花的优劣. 结果表明不同金银花提取物(M1, M2, Z1, Z2)的¹³C NMR指纹图谱都显示出绿原酸的特征共振峰,并具有很好的重现性和高度的特征性,可以成为金银花真伪鉴别的依据;优质(M1, Z1)与劣质(劣质M1,劣质Z1)金银花¹³C NMR图谱的差异进一步说明¹³C NMR指纹图谱可作为鉴别金银花质量的依据.     

HPTLC and ATR/FTIR Characterization of Antioxidants in Different Rosemary Extracts

The effect of spontaneous fermentation by lactic acid bacteria on the extraction yield of bioactive compounds and antioxidant activity from rosemary leaf extracts was investigated using high-performance thin-layer chromatography (HPTLC). Brining and spontaneous fermentation with lactic acid bacteria more than doubled extraction of polyphenolics and antioxidants from the rosemary leaves. The results show that lactic acid fermentation enhances antioxidant activity in extracts by increasing the total phenolic content but does not increase extraction of phytosterols. Increased extraction of phenolic oxidants during fermentation assisted extraction, results from the in situ generated natural eutectic solvent from the plant sample. ATR-FTIR spectra from the bioactive bands suggests that this increased antioxidant activity is associated with increased extraction of rosmarinic acid, depolymerised lignin, abietane diterpenoids and 15-hydroxy-7-oxodehydroabietic acid.