An approach to comparative analysis of chromatographic fingerprints for assuring the quality of botanical drugs

The present study was focused on developing the chemometric methods for analysis of the chromatographic fingerprint to control the quality of botanical drugs, which has gained attention in Asia and other countries. We developed a novel approach to generate a set of fingerprint features, called Fisher components (FCs) that were extracted from the chromatographic fingerprint. The method greatly reduces the dimensionality of the fingerprint vector, and the resulting FCs still retain most discriminatory information of the original fingerprint. Choosing an example of relevance to contemporary botanical drugs, we applied the FCs to a set of Shenmai injection samples. We successfully identified the manufacturers of the samples using two classifiers, linear discriminant analysis (LDA) and k-Nearest Neighbor (k-NN) based on the FCs. We also applied a similarity assessment together with the visual analysis using the FCs to exam the products from different manufacturers. We found that the lot-to-lot consistency of products can be accurately determined using the FCs. Finally, we demonstrated that the application of chemometric methods for chromatographic fingerprinting offers reliability to detect suspected fraud samples. In summary, we demonstrated that the presented approaches could be useful to determine the identity, consistency, and authenticity of Shenmai injection through chromatographic fingerprinting. The methods are equally applicable to other botanical drugs.     

On-line identification of phytochemical constituents in botanical extracts by combined high-performance liquid chromatographic-diode array detection-mass spectrometric techniques

It is necessary to determine all of the phytochemical constituents of botanical extracts in order to ensure the reliability and repeatability of pharmacological and clinical research, to understand their bioactivities and possible side effects of active compounds and to enhance product quality control. HPLC chromatographic fingerprints can be applied for this kind of documentation. Combined HPLC-diode array detection–MS techniques can provide on-line UV and MS information for each peak in a chromatogram. In most cases, direct identification of the peaks is possible, based on comparison with published data or with standard compounds. This review will primarily focus on electrospray and thermospray ionization MS and their applications for the qualitative analyses of phenolic compounds, saponins, alkaloids and other classes of natural products in botanical extracts. Twenty-one of the most commonly used herbal examples, their phytochemical analyses and characteristics of their mass spectra are described.     

Application and efficiency of thermal analysis in a production laboratory

The application of thermoanalytical methods to technical products in a production laboratory is characterised by a close connection with the specific production process and therefore it is frequently confronted with a large variety of samples. Contrary to research laboratories there are almost no pure material systems to be tested. This means that in harsh environments thermoanalytical methods must provide results with high sensitivity and reproducibility in order to detect reacting components. The example of technical plastics shows not only the efficiency but also the problems of Thermal Analysis for materials testing. Discussed are polyethylene for cable insulation and for pipes, and epoxy resins for injection moulded parts in the electrical engineering field. Demonstrated is the routine application of DSC to determine the crystallinity, curing, and oxydation stability. TG to determine the temperature stability and TMA to measure the degree of curing. A comparison is made between results obtained from different Thermal Analysis methods.     

Recent studies on selected botanical dietary supplement ingredients

The market for botanical dietary supplements in the US has grown rapidly during the last 15 years. Use of newly introduced botanical ingredients has often outpaced an adequate scientific understanding of the ingredients themselves. This may lead to problems, including misidentification, mislabeling, adulteration, and toxicity related to the intended ingredient or one substituted for it. This article reviews recent work with several botanical ingredients (Ephedra, Citrus species, Hoodia gordonii, Teucrium, isoflavones) that illustrates the complexity of the current situation and approaches that contribute to ensuring the quality of botanical ingredients. Recent work with contamination of botanical products by mycotoxins is also reviewed. The need for tools for botanical authentication and methods for reproducible extraction of bioactive constituents is critical. Such tools, and improved analytical techniques for identifying potentially bioactive constituents in fresh plant material and in concentrated extracts and for detection of hazardous contaminants, are expected to improve the overall quality and safety of botanical dietary supplement ingredients.     

Methodology in internal quality control of chemical analysis

Internal quality control (IQC) is an essential feature of routine analysis, serving to ensure that the uncertainty of results found during the validation of a procedure is maintained over long periods of time. The primary method of IQC is to analyse a surrogate material alongside the test materials in every run of analysis and thus address run-to-run precision (a subset of VIM3-defined ‘intermediate conditions’). This ‘control material’ must be as similar as practicable in composition to the routine test materials, although there are always some differences. Results from the control material (control values) are plotted on a control chart, and out-of-control results have to be investigated and problems rectified. Considerable care is needed in obtaining correct values of the parameters for determining statistical control limits, and these can be adequately estimated only during routine use of the analytical procedure. In contrast, target control limits have to be set on a fitness-for-purpose basis and are necessarily wider that statistical control limits. An additional type of internal quality control can be executed by the analysis of duplicate test portions of some of the actual test samples. This provides a realistic dispersion, but addresses only repeatability precision. A further complication of duplication is that the precision of results typically varies with concentration of the analyte.     

Degradation issues of polymer materials used in railway field

Polymer materials used in railway field are degraded by environmental factors such as thermal, oxidative, photolytic, hydrolytic, and mechanical. The expected service life of the polymer materials used in railway field is approximately 20 years that is relatively long period for the polymer material; therefore, respective degradation factors should be well considered. Some of the degradation conditions indicate similar mechanism. The oxidative reaction was seen in every degradation conditions under air atmosphere. The hydrolytic reaction was mainly observed in chemical and biological degradations. The degradation behavior of the polymer material was analyzed by various methods. FTIR, thermal analysis (TG, DSC), and molecular weight determination were mainly applied for its purpose. However, the degradation mechanism of practical products made of polymer material was insufficiently studied and the exchange criteria of the products depended on the visual inspection without the suitable degradation analysis not only in the railway field but also in other commercial and industrial fields. In addition, most of the methods to analyze degradation of polymer material are performed on the standard specimen forms. For the installed product, some kinds of damage are generated through the sample collection process; therefore, the damaged products have to be exchanged for brand new ones or repaired totally to be used for more period. Moreover, it is hard to suspend the railway service for the degradation analysis of polymer products. From these backgrounds, the prospect of degradation analysis related to polymer materials used in railway field was proposed.     

Applications of sol-gel technology in imaging

New materials need to be developed to fulfill the future requirements of the imaging business. This applies to the development of new products, but also to the improvement of current products of processes in different areas such as image capture, storage, manipulation, display or printing. Examples of such materials based on sol-gel technology are given, including conductive oxides for antistatic films, sensors or membranes for environmental applications and optical films. For each example specific key issues have to be addressed, so that the material can be used in real applications.     

Natural resins and balsams from an eighteenth-century pharmaceutical collection analysed by gas chromatography/mass spectrometry

Historical nomenclature has not always been unequivocally associated with the botanical origin of natural resins. The availability of natural resins has changed throughout the centuries and so have their trade names. Furthermore, adulterations and lack of knowledge have led to variations in the composition of the products traded under the same name. This investigation aims at a new understanding of the interrelation between the historical and modern terms for natural resins. Different Pinaceae and Pistacia resins, mastic, sandarac, copaiba balm and burgundy pitch from Vigani’s Cabinet, a 300-year-old pharmaceutical collection owned by Queens’ College, Cambridge (UK) were investigated. Related reference materials from modern collections were analysed together with natural resins derived from reliable botanical sources. The analytical method was gas chromatography/mass spectrometry (GC-MS) with and without derivatisation with trimethylsulfonium hydroxide. This technique provided detailed molecular compositions of the studied materials, which in turn led to particular data profiles of the materials. Marker molecules of Copaifera, Pinaceae, Cupressaceae and Pistacia resins were identified. By comparing the GC-MS data profiles to the reference samples, a clearer picture of the connection between nomenclature and botanical origin was obtained. With the aid of the marker molecules and data profiles, it was then possible to clarify the nomenclature of the aged resins sampled from Vigani’s Cabinet.     

Reference materials – an industry perspective

Biotechnologically enhanced plants and products derived thereof continue to be the reason for much dispute. In order to address concerns raised by the public, several countries have imposed mandatory labeling schemes indicating the presence of products derived from modern biotechnology, while others rely on voluntary labeling codes. Mandatory labeling triggers the need for methods that can be used to check compliance with and enforcement of the corresponding labeling legislation. In order to ensure the proper validation and implementation of a detection method in a specific laboratory, reference materials play a crucial role.Electronic Supplementary Material Supplementary material is available for this article if you access the article at . A link in the frame on the left on that page takes you directly to the supplementary material.Presented at the CCQM Workshop on Comparability and Traceability in Food Analysis, 18–19 November 2003, BIPM, Sèvre, France.     

Characterization of a suite of ginkgo-containing standard reference materials

A suite of three ginkgo-containing dietary supplement Standard Reference Materials (SRMs) has been issued by the National Institute of Standards and Technology (NIST) with certified values for flavonoid aglycones, ginkgolides, bilobalide, and selected toxic trace elements. The materials represent a range of matrices (i.e., plant, extract, and finished product) that provide different analytical challenges. The constituents have been determined by at least two independent analytical methods with measurements performed by NIST and at least one collaborating laboratory. The methods utilized different extractions, chromatographic separations, modes of detection, and approaches to quantitation. The SRMs are primarily intended for method validation and for use as control materials to support the analysis of dietary supplements and related botanical materials. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Application of the Metabolomics Approach in Food Authentication

The authentication of food products is essential for food quality and safety. Authenticity assessments are important to ensure that the ingredients or contents of food products are legitimate and safe to consume. The metabolomics approach is an essential technique that can be utilized for authentication purposes. This study aimed to summarize food authentication through the metabolomics approach, to study the existing analytical methods, instruments, and statistical methods applied in food authentication, and to review some selected food commodities authenticated using metabolomics-based methods. Various databases, including Google Scholar, PubMed, Scopus, etc., were used to obtain previous research works relevant to the objectives. The review highlights the role of the metabolomics approach in food authenticity. The approach is technically implemented to ensure consumer protection through the strict inspection and enforcement of food labeling. Studies have shown that the study of metabolomics can ultimately detect adulterant(s) or ingredients that are added deliberately, thus compromising the authenticity or quality of food products. Overall, this review will provide information on the usefulness of metabolomics and the techniques associated with it in successful food authentication processes, which is currently a gap in research that can be further explored and improved.     

Evaluation of botanical reference materials for the determination of vanadium in biological samples

Three botanical reference materials prepared by the National Bureau of Standards have been studied by neutron activation analysis to evaluate their suitability with respect to the determination of vanadium in biological samples. Various decomposition methods were applied in connection with chemical or radiochemical separations, and results for vanadium were compared with those found by purely instrumental neutron activation analysis. Significantly lower results indicate losses or incomplete dissolution, which makes SRM 1575 Pine Needles and SRM 1573 Tomato Leaves less satisfactory than SRM 1570 Spinach. A reference value of 1.15 mg/kg of this material is recommended, based on results from 3 different methods. All three materials are preferable to SRM 1571 Orchard Leaves, while Bowen's Kale remains the material of choice because of its lower concentration.     

Production and certification of “fresh” reference material for macronutrient analysis

Summary Reference materials for carrying out in-house quality assurance by food laboratories that analyse macronutrients have to date been inadequate. The freeze-dried, very specialized, materials that exist on the market are not always comparable with ordinary food products analysed at those laboratories.A homogeneous, fresh, canned meat material was produced by an ordinary cannery. The total amount of material (pork, nitrite salt and water) was 1700 kg. During production, the fat content was continuously analysed in the different sub-batches and combinations are made accordingly. The material was packed in tin cans containing 200 g, and tested for homogeneity. The shelf life is, by experience, at least five years. A large number of authorized public and industry laboratories participated in the certification procedure. For each constituent different types of standard analytical methods were used. The material is offered for sale together with a certificate, giving mean values for moisture, ash, fat, nitrogen, sodium, sodium chloride and hydroxyproline content. The uncertainty is given as standard deviations including the analytical error and the variations between laboratories, methods and units.     

High-performance liquid chromatography/mass spectrometry analysis of botanical medicines and dietary supplements: a review

This article reviews research on the qualitative and quantitative analysis by high-performance column liquid chromatography/mass spectrometry (LC/MS) and LC/tandem mass spectrometry (LC/MS/MS) of botanical drugs, drug substances or preparations, and finished botanical products. In addition, LC/MS and LC/MS/MS techniques and commercial instruments are described and compared briefly, and prospects for future use of these methods for the analysis of botanicals are suggested. Some applications of direct MS without LC are also described.     

The Cradle-to-Cradle Life Cycle Assessment of Polyethylene terephthalate: Environmental Perspective

Over the last several years, the number of concepts and technologies enabling the production of environmentally friendly products (including materials, consumables, and services) has expanded. One of these ways is cradle-to-cradle (C2C) certified^TM. Life cycle assessment (LCA) technique is used to highlight the advantages of C2C and recycling as a method for reducing plastic pollution and fossil depletion by indicating the research limitations and gaps from an environmental perspective. Also, it estimates the resources requirements and focuses on sound products and processes. The C2C life cycle measurements for petroleum-based poly (ethylene terephthalate) (PET) bottles, with an emphasis on different end-of-life options for recycling, were taken for mainland China, in brief. It is considered that the product is manufactured through the extraction of crude oil into ethylene glycol and terephthalic acid. The CML analysis method was used in the LCIA for the selected midpoint impact categories. LCA of the product has shown a drastic aftermath in terms of environmental impacts and energy use. But the estimation of these consequences is always dependent on the system and boundary conditions that were evaluated throughout the study. The impacts that burden the environment are with the extraction of raw material, resin, and final product production. Minor influences occurred due to the waste recycling process. This suggests that waste degradation is the key process to reduce the environmental impacts of the production systems. Lowering a product’s environmental impact can be accomplished in a number of ways, including reducing the amount of materials used or choosing materials with a minimal environmental impact during manufacture processes.     

New liquid chromatography method with ultraviolet detection for analysis of anthocyanins and anthocyanidins in Vaccinium myrtillus fruit dry extracts and commercial preparations

The Vaccinium myrtillus fruits (bilberry) are a well-known anthocyanins source, and their extracts are widely used in dietary botanicals and pharmaceutical products for the treatment of vascular and vision disorders. Different analytical methods used for standardization of the bilberry extracts and their preparations are available from pharmacopeias and from the literature. However, the methods reported in the literature do not allow the detection of free anthocyanidins, which are markers of poor product quality. A new liquid chromatography method was developed and validated for the identification and quantification of both anthocyanins and anthocyanidins present in bilberry extracts and products. The method shows a good reproducibility and, due to its high specificity, is suitable to identify unequivocally the botanical raw materials used for manufacturing and to evaluate the extract composition, thus ensuring a high degree of product consistency and quality. Forty typical bilberry preparations belonging to 24 different brands were purchased in the marketplace and evaluated for their quality by using the developed method. Results revealed marked differences among the brands despite a common origin and labeling.     

Die Verfügbarkeit von Hochtechnologie‐Rohstoffen

It is vital to ensure that the German economy is supplied with the mineral resources that it needs. In 2010, the Ad‐Hoc Working Group on defining critical raw materials of the European Commission has identified 14 materials as critical. Although the task of securing the supply of raw materials is with the industry, both the German government and the European Union have defined strategies for future‐oriented and sustainable raw materials supply. The establishment of the German Mineral Resources Agency (DERA) as a central information centre for the industry is part of the German Government's raw materials strategy. The reserves of most critical raw materials are considered large enough to meet the demand of years to come. In addition, there are numerous options of substitution, recycling and of recovering metals from non‐used deposits. However, it is a combination of factors such as the geological availability, geostrategic risks and market power that result in an assessment as a critical raw material. These factors have to be taken into account by the industry to be able to effectively react to changing market situations. In this respect, the future development of the BRIC countries, led by China, is considered most important. Due to the growing industrialization, their raw materials consumption increases; furthermore, technologies using critical raw materials for domestic production are being developed. In such resource‐rich countries, export capacities of certain critical materials are being reduced and thus import prices tend to increase. Pressure on raw material producers outside of these countries is growing. Consequently, raw materials are increasingly sourced from regions that do not meet criteria of sustainable mining practice, environmental management and social security, as seen for example in many artisanal mining operations. Furthermore, in some countries mining is related to violent conflicts. In the future, both consumers and industry will increasingly ask for the implementation of minimum standards in artisanal mining and of transparency in mineral supply chains.     

Recent developments in NIST botanical SRMs

The National Institute of Standards and Technology (NIST) (formerly the National Bureau of Standards (NBS)) issued the first botanical reference material certified for elemental content in January 1971, as Standard Reference Material (SRM) 1571, Orchard Leaves. In the following years a total of nine additional botanical certified reference materials have been issued by NIST. Each of these materials was certified for major, minor and trace elements except for SRM 2695, certified for fluorine only. Botanical SRMs issued since 1991 are significantly improved over previous materials in a number of ways. Probably the most significant change is the use of a jet-milling process to grind them to extremely fine particles. This has resulted in botanical SRMs with significantly improved homogeneity. These NIST reference materials are described with information on homogeneity, drying techniques and grit content.