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Quality control in pharmaceutical manufacturing necessitates rigorous testing and approval, adhering to Current Good Manufacturing Practices before commercialization. The production of solid drugs presents significant industrial challenges regarding uniformity, homogeneity, and consistency. Traditional quality guidelines rely on classical analytical methods such as liquid chromatography coupled with mass spectrometry. However, the emergence of Process Analytical Technology introduced non-destructive, rapid, and cost-effective methods like UV-Visible Diffuse Reflectance Spectroscopy. The present study aimed to develop a chemometric method for quantifying Active Pharmaceutical Ingredients (APIs) in Neo Nisidine®, a solid mixture drug, using spectrophotometric data. The Net Analyte Signal (NAS) method, combined with standard additions, allowed the creation of a pseudo-univariate standard addition model, overcoming some challenges in solid-phase analysis. Successful quantifications of APIs in ideal laboratory samples and real pharmaceutical tablets were obtained. NAS-based chemometric models showed high precision and reliability, whose results were validated by comparisons with HPLC ones. The study revealed that solid-phase spectrophotometric analyses can be considered a valid alternative to API analyses. Solid-phase analysis offers non-destructive, cost-effective, and environmentally friendly benefits, enabling its integration into pharmaceutical production to improve quality control. [ABSTRACT FROM AUTHOR]

A novel approach for the quantification of recycled polyethylene terephthalate (r-PET) in commercial bottles is presented. Fifty-eight bottle samples from several brands and producers containing different percentages of r-PET were purchased from the market. Samples were analyzed by two spectroscopic methods: near-infrared (NIR) spectroscopy and attenuated total reflection (ATR) spectroscopy in the mid-infrared (MIR) region. No chemical pre-treatment was applied before analyses. The spectra were analyzed by partial-least squares (PLS) regression, and two models for NIR and MIR data were computed. Then, a multi-block regression was applied to join the two datasets. All models were validated by cross-validation and by excluding and projecting onto the model the replicated spectra of one sample at a time. Results demonstrated the potential of this approach, especially considering the variability of commercial samples in terms of additives, shape, or thickness of the bottles: for samples close to the centroids of the models (i.e., from 10 to 50% r-PET), the predictions of multi-block method seldom departed from the expected values of ±10%. Only for samples with 0% declared r-PET, the models showed poor prediction abilities. [ABSTRACT FROM AUTHOR]

In the last 20 years, an increased interest has been shown in the application of different types and combinations of enzymes to obtain phenolic extracts from grape pomace in order to maximize its valorization. Within this framework, the present study aims at improving the recovery of phenolic compounds from Merlot and Garganega pomace and at contributing to the scientific background of enzyme-assisted extraction. Five commercial cellulolytic enzymes were tested in different conditions. Phenolic compound extraction yields were analyzed via a Design of Experiments (DoE) methodology and a second extraction step with acetone was sequentially added. According to DoE, 2% w/w enzyme/substrate ratio was more effective than 1%, allowing a higher total phenol recovery, while the effect of incubation time (2 or 4 h) variation was more enzyme-dependent. Extracts were characterized via spectrophotometric and HPLC-DAD analyses. The results proved that enzymatic and acetone Merlot and Garganega pomace extracts were complex mixtures of compounds. The use of different cellulolytic enzymes led to different extract compositions, as demonstrated using PCA models. The enzyme effects were observed both in water enzymatic and in the subsequent acetone extracts, probably due to their specific grape cell wall degradation and leading to the recovery of different molecule arrays. [ABSTRACT FROM AUTHOR]

Instrument automation, technological advancements and improved computational power made separation science an extremely data-rich approach, requiring the use of statistical and data analysis tools that are able to optimize processes and combine multiple outputs. The use of chemometrics is growing, greatly improving the ability to extract meaningful information. Separation–multidetection generates multidimensional data, whose elaboration should not be left to the discretion of the operator. However, some applications or techniques still suffer from the lack of method optimization through DoE and downstream multivariate analysis, limiting their potential. This review aims at summarizing how chemometrics can assist analytical chemists in terms of data elaboration and method design, focusing on what can be achieved by applying chemometric approaches to separation science. Recent applications of chemometrics in separation analyses, in particular in gas, liquid and size-exclusion chromatography, together with field flow fractionation, will be detailed to visualize the state of the art of separation chemometrics, encompassing volatile, soluble and solid (colloidal) analytes. The samples considered will range from food chemistry and environmental chemistry to bio/pharmaceutical science. [ABSTRACT FROM AUTHOR]

Tomato sauce is a world famous food product. Despite standards regulating the production of tomato derivatives, the market suffers frpm fraud such as product adulteration, origin mislabelling and counterfeiting. Methods suitable to discriminate the geographical origin of food samples and identify counterfeits are required. Chemometric approaches offer valuable information: data on tomato sauce is usually obtained through chromatography (HPLC and GC) coupled to mass spectrometry, which requires chemical pretreatment and the use of organic solvents. In this paper, a faster, cheaper, and greener analytical procedure has been developed for the analysis of volatile organic compounds (VOCs) and the colloidal fraction via multivariate statistical analysis. Tomato sauce VOCs were analysed by GC coupled to flame ionisation (GC-FID) and to ion mobility spectrometry (GC-IMS). Instead of using HPLC, the colloidal fraction was analysed by asymmetric flow field-fractionation (AF4), which was applied to this kind of sample for the first time. The GC and AF4 data showed promising perspectives in food-quality control: the AF4 method yielded comparable or better results than GC-IMS and offered complementary information. The ability to work in saline conditions with easy pretreatment and no chemical waste is a significant advantage compared to environmentally heavy techniques. The method presented here should therefore be taken into consideration when designing chemometric approaches which encompass a large number of samples. [ABSTRACT FROM AUTHOR]

Bioindicator plants are species that have the capacity to linearly uptake some elements (metal and metalloids) from the growing substrate, thus reflecting their concentration in the soil. Many factors can influence the uptake of these elements by plants, among which is the simultaneous presence of several metals, a common situation in contaminated or natural soils. A novel approach that can be used to validate the bioindication ability of a species growing on a polymetallic substrate is the design of experiment (DoE) approach. The aim of the present study was to apply the DoE in full factorial mode to model the Cu, Cd, Pb, Zn, and Cr bioindication capacity of Polygonum aviculare, used as the model plant. The results showed that P. aviculare has the ability to bioindicate Cd and Cr with a linear uptake (from 0.35 to 6.66, and 0.1 to 3.4 mg kg−1, respectively) unaffected by the presence of other metals. Conversely, the uptake of Pb, Cu, and Zn is strongly influenced by the presence of all the studied metals, making their concentration in the plant shoot not proportional to that of the soil. In conclusion, these preliminary results confirmed that the DoE can be used to predict the bioindicator abilities of a plant for several elements at the same time and to evaluate the interactions that can be established between variables in the growing medium and in the plant itself. However, more studies including other plant species are needed to confirm the effectiveness of this method. [ABSTRACT FROM AUTHOR]

The present paper reports a new application: the voltammetric determination in herbal medicines of ultra-trace thallium(I), in the presence of lead(II), tin(II) and antimony(III) as interfering metals, by square wave anodic stripping voltammetry (SWASV). A conventional three-electrodes voltammetric cell was employed with a stationary hanging mercury drop electrode (HMDE) as working electrode and a platinum electrode and an Ag|AgCl|KClsatd. electrode as auxiliary and reference electrodes, respectively. The supporting electrolyte was 0.5 mol L􀀀1 ammonium citrate buffer pH 6.5 + 7.3 10􀀀3 mol L􀀀1 EDTA-Na2. The analytical procedure was verified by the analysis of the standard reference materials: spinach Leaves NIST-SRM 1570a and tomato leaves NIST-SRM 1573a from National Institute of Standards and Technology. Precision and trueness, expressed as relative standard deviation and relative error, respectively, were generally lower than 7% in all cases. Once set up on the standard reference materials, the analytical procedure was transferred and applied to herbal medicines samples--Taraxacun officinale weber, Eucalyptus globulus and Harpagophytum procumbens DC--sold on the market. A critical comparison with spectroscopic measurements is also discussed. [ABSTRACT FROM AUTHOR]

An authenticity study on Italian grape marc spirit was carried out by gas chromatography (GC) and chemometrics. A grape marc spirit produced in Italy takes the particular name of "grappa", a product which has peculiar tradition and production in its country of origin. Therefore, the evaluation of its authenticity plays an important role for its consumption in Italy, as well as for its exportation all around the world. For the present work, 123 samples of grappa and several kinds of spirits were analyzed in their alcohol content by electronic densimetry, and in their volatile fraction by gas-chromatography with a flame-ionization detector. Part of these samples (94) was employed as a training set to compute a chemometric model (by linear discriminant analysis, LDA) and the other part (29 samples) was used as a test set to validate it. Finally, two grappa samples seized from the market by the Italian Customs and Monopolies Agency and considered suspicious due to their aroma reported as non-compliant were projected onto the LDA model to evaluate the compliance with the "grappa" class. A further one-class classification method by principal component analysis (PCA) was carried out to evaluate the compliance with other classes. Results showed that the suspicious samples were not recognized as belonging to any of the analyzed spirit classes, confirming the starting hypothesis that they could be grappa samples adulterated in some way. [ABSTRACT FROM AUTHOR]

The present study aims to highlight the therapeutic potential of Asphodeline lutea (AL), a wild edible plant of the Mediterranean diet. Roots, aerial parts, and flowers of AL at two different phenological stages were collected from three locations in Italy. The inhibitory activities of extracts on strategic enzymes linked to human diseases were assessed. The antioxidant properties were evaluated in vitro, using six standard bioassays. The phenolic and anthraquinone profiles were also established using HPLC-PDA. Zinc, cadmium, lead, and copper contents were also determined. All the samples inhibited acetylcholinesterase (from 1.51 to 2.20 mg GALAEs/g extract), tyrosinase (from 7.50 to 25.3 mg KAEs/g extract), and α-amylase (from 0.37 to 0.51 mmol ACAEs/g extract). Aloe-emodin and physcion were present in all parts, while rhein was not detected. The phenolic profile and the heavy metals composition of specimens gathered from three different regions of Italy were different. It can be argued that samples collected near the street can contain higher concentrations of heavy metals. The experimental data confirm that the A. lutea species could be considered as a potential source of bioactive metabolites, and its consumption could play a positive and safe role in human health maintenance. [ABSTRACT FROM AUTHOR]

The international seafood trade is based on food safety, quality, sustainability, and traceability. Mussels are bio-accumulative sessile organisms that need regular control to guarantee their safe consumption. However, no well-established and validated methods exist to trace mussel origin, even if several attempts have been made over the years. Recently, an inorganic multi-elemental fingerprint coupled to multivariate statistics has increasingly been applied in food quality control. The mussel shell can be an excellent reservoir of foreign inorganic chemical species, allowing recording long-term environmental changes. The present work investigates the multi-elemental composition of mussel shells, including Al, Cu, Cr, Zn, Mn, Cd, Co, U, Ba, Ni, Pb, Mg, Sr, and Ca, determined by inductively-coupled plasma mass-spectrometry in Mytilus galloprovincialis collected along the Central Adriatic Coast (Marche Region, Italy) at 25 different sampling sites (18 farms and 7 natural banks) located in seven areas. The experimental data, coupled with chemometric approaches (principal components analysis and linear discriminant analysis), were used to create a statistical model able to discriminate samples as a function of their production site. The LDA model is suitable for achieving a correct assignment of >90% of individuals sampled to their respective harvesting locations and for being applied to counteract fraud. [ABSTRACT FROM AUTHOR]

This study was conducted to develop systems for the identification of four tuna species (skipjack tuna Katsuwonus pelamis, yellowfin tuna Thunnus albacares, bullet tuna Auxis sp. and Atlantic bonito Sarda sp). At first, raw samples of these species and a mix intended as internal control were prepared for the authentication of fish muscle tissue of the genus Thunnus sp., Auxis sp. and Sarda sp. DNA from raw muscle tissue, the mix and samples was extracted with the DNeasy mericon Food Kit (Qiagen GmbH, Hilden, Germany). The concentration and purity of DNA in raw samples were evaluated using a spectrophotometer. Primers and probe sequences were specifically designed to identify the selected species. In addition, primers and a probe for the endogenous 12S rRNA gene were designed to determine the presence of amplifiable fish (especially tuna) DNA in samples. Furthermore, the species specificity of the designed primers and probes was verified in DNA samples of various tuna and bonito species. Limit of detection for the selected species was calculated as well as the coefficient of determination R2 and efficiency of real-time PCR testing was determined. To evaluate the developed real-time PCR methods, 70 commercial tuna products were analysed. The results show that mislabelling of fish products can still be encountered and, moreover, the presence of an additional species can be identified. [ABSTRACT FROM AUTHOR]

Alternaria toxins are emerging mycotoxins whose regulation and standardization are in progress by the European Commission and the European Committee for Standardization. This paper describes a dilute and shoot approach to determine five Alternaria toxins in selected food samples using liquid chromatography–tandem mass spectrometry (LC-MS/MS). The strategy involves sample extraction with acidified aqueous methanol, followed by a solvent change accomplished via sample evaporation and reconstitution. The quantification is based on isotope dilution, applying all corresponding isotopically labeled internal standards to compensate possible matrix effects of the analysis. The main advantages of the present method over other existing methods includes simple and effective sample preparation, as well as detection with high sensitivity. The five-fold sample dilution can decrease matrix effects, which were evaluated with both external and internal standard methods. The results demonstrated a limit of quantification lower than 1.0 µg/kg for all five analytes for the first time. The newly presented method showed acceptable accuracy (52.7–111%) when analyzing naturally contaminated and spiked standard samples at the described levels. The method was validated for tomato-based and flour samples (wheat, rye, and maize). The absolute recovery ranged from 66.7% to 91.6% (RSD < 10%). The developed method could be an alternative approach for those laboratories that exclude sample cleanup and pre-concentration of state-of-the-art instruments with enhanced sensitivity. [ABSTRACT FROM AUTHOR]

We developed a method for determination of imidacloprid and its metabolites 5-hydroxy imidacloprid, olefin imidacloprid, imidacloprid urea and 6-chloronicotinic acid in Procambarus clarkii (crayfish) tissues using quick, easy, cheap, effective, rugged, and safe (QuEChERS) and high-performance liquid chromatography-triple quadrupole mass spectrometry. Samples (plasma, cephalothorax, hepatopancrea, gill, intestine, and muscle) were extracted with acetonitrile containing 0.1% acetic acid and cleaned up using a neutral alumina column containing a primary secondary amine. The prepared samples were separated using reverse phase chromatography and scanned in the positive and negative ion multiple reaction-monitoring modes. Under the optimum experimental conditions, spiked recoveries for these compounds in P. clarkii samples ranged from 80.6 to 112.7% with relative standard deviations of 4.2 to 12.6%. The limits of detection were 0.02–0.5 μg·L−1, the limits of quantification were 0.05–2.0 μg·L−1 and the method of quantification was 0.05–2.0 μg·kg−1. The method is rapid, simple, sensitive and suitable for rapid determination and analysis of imidacloprid and its metabolites in P. clarkii tissues. [ABSTRACT FROM AUTHOR]

Plants growing on heavy metal (HM)-polluted soils show toxicity symptoms, such as chlorosis and growth reduction, and undergo oxidative stress due to the formation of reactive oxygen species (ROS). Plants overcome oxidative stress by producing a wide range of antioxidant molecules, such as polyphenols and flavonoids. The aim of the present work was to study the accumulation of these molecules in response to increasing concentrations of Cd, Cr, Cu, Ni, Pb and Zn and to assess whether they can be used as a tool in assessing metal-related stress in Polygonum aviculare and Senecio vulgaris. On average, P. aviculare shoots accumulated lower amounts of metals than S. vulgaris shoots. The uptake of all six elements was correlated and proportional to their concentration in the nutrient solution (ρ > 0.9), with the bioaccumulation factor (BAF) being >1 for most of them. The present research demonstrated that 82% of the samples showed a good correlation (|ρ| > 0.5) between the level of polyphenols, flavonoids and antioxidant activity and the metal concentration in plant shoots, confirming that the metal stress level and production of phenolic compounds having antioxidant activity were strictly connected. Nonetheless, the mere quantification of these molecules cannot identify the type of metal that caused the oxidative stress, neither determine the concentration of the stressors. The five tested populations of each species did not show any specific adaptation to the environment of origin. [ABSTRACT FROM AUTHOR]

Surface pollution deposition in a high voltage surface can reduce the surface flashover voltage, which is considered to be a serious accident in the transmission of electric power for the high conductivity of pollution in wet weather, such as rain or fog. Accordingly, a rapid and accurate online pollution detection method is of great importance for monitoring the safe status of transmission lines. Usually, to detect the equivalent salt deposit density (ESDD) and non-soluble deposit density (NSDD), the pollution should be collected when power cut off and bring back to lab, time-consuming, low accuracy and unable to meet the online detection. Laser-induced breakdown spectroscopy (LIBS) shows the highest potential for achieving online pollution detection, but its application in high voltage electrical engineering has only just begun to be examined. In this study, a LIBS method for quantitatively detecting the compositions of pollutions on the insulators was investigated, and the spectral characteristics of a natural pollution sample were examined. The energy spectra and LIBS analysis results were compared. LIBS was shown to detect pollution elements that were not detected by conventional energy spectroscopy and had an improved capacity to determine pollution composition. Furthermore, the effects of parameters, such as laser energy intensity and delay time, were investigated for artificial pollutions. Increasing the laser energy intensity and selecting a suitable delay time could enhance the precision and relative spectral intensities of the elements. Additionally, reducing the particle size and increasing the density achieved the same results. [ABSTRACT FROM AUTHOR]

Volatile organic compounds (VOCs) in wood furniture are an important factor that affects indoor air quality. In this study, radiata pine (Pinus radiata D. Don) was treated with sodium bicarbonate and ozone aqueous solution to reduce the VOC contents without sacrificing mechanical properties. The VOCs of radiata pine were identified by gas chromatography-mass spectrometry (GC-MS), and the functional group changes of wood samples were characterized by Fourier-transform infrared spectroscopy (FTIR). The results showed that the main VOCs of radiata pine include alkenes, aldehydes, and esters. The sodium bicarbonate and ozone treatments almost eliminated the VOC contents of radiata pine. The two treatments mentioned above had little effect on compressive strength and surface color of radiata pine. [ABSTRACT FROM AUTHOR]

(1) Background: Flavonoids are the primary medicinal ingredient of Saussurea involucrate, which have significant antioxidant capacity. Optimizing the extraction of Saussurea involucrate flavonoids (SIFs) and exploring the ability to block melanin deposition caused by reactive oxygen can greatly promote the development of S. involucrate whitening products. (2) Methods: Ultrasonic extraction process was optimized using the Box–Behnken design (BBD) and response surface methodology (RSM). Then, the effect of SIFs on antioxidant activity and anti-deposition of melanin, and genes related to the melanin synthesis are studied. (3) Results: The optimal extraction procedures are as follows: the extraction time, ethanol content, and solvent ratio (v/w) are 64 min, 54%, and 54:1, respectively. The reducing activity and scavenging rates of 2,2-diphenyl-1-picrylhydrazyl (DPPH), superoxide anion, hydroxyl radical, and ABTS+ were promoted as more S. involucrate flavonoid extract was added. The SIFs extract induced a decrease in the melanin synthesis by inhibiting the human melanoma A375 cell tyrosinase activity. SIFs also depress expression of melanin synthesis related genes. (4) Conclusions: the highest SIFs content was obtained by using 54% ethanol and 54:1 solvent ratio (v/w) for 64 min. The extract of SIFs exhibited good ability of antioxidant and anti-deposition of melanin in human melanocytes. [ABSTRACT FROM AUTHOR]

Biogenic silica is the major component of the external skeleton of marine micro-organisms, such as diatoms, which, after the organisms death, settle down onto the seabed. These micro-organisms are involved in the CO2 cycle because they remove it from the atmosphere through photosynthesis. The biogenic silica content in marine sediments, therefore, is an indicator of primary productivity in present and past epochs, which is useful to study the CO2 trends. Quantification of biosilica in sediments is traditionally carried out by wet chemistry followed by spectrophotometry, a time-consuming analytical method that, besides being destructive, is affected by a strong risk of analytical biases owing to the dissolution of other silicatic components in the mineral matrix. In the present work, the biosilica content was directly evaluated in sediment samples, without chemically altering them, by attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy. Quantification was performed by combining the multivariate standard addition method (MSAM) with the net analyte signal (NAS) procedure to solve the strong matrix effect of sediment samples. Twenty-one sediment samples from a sediment core and one reference standard sample were analyzed, and the results (extrapolated concentrations) were found to be comparable to those obtained by the traditional wet method, thus demonstrating the feasibility of the ATR-FTIR-MSAM-NAS approach as an alternative method for the quantification of biosilica. Future developments will cover in depth investigation on biosilica from other biogenic sources, the extension of the method to sediments of other provenance, and the use higher resolution IR spectrometers. [ABSTRACT FROM AUTHOR]

Extracellular vesicles (EVs) are lipid bilayer enclosed particles which present in almost all types of biofluids and contain specific proteins, lipids, and RNA. Increasing evidence has demonstrated the tremendous clinical potential of EVs as diagnostic and therapeutic tools, especially in biofluids, since they can be detected without invasive surgery. With the advanced mass spectrometry (MS), it is possible to decipher the protein content of EVs under different physiological and pathological conditions. Therefore, MS-based EV proteomic studies have grown rapidly in the past decade for biomarker discovery. This review focuses on the studies that isolate EVs from different biofluids and contain MS-based proteomic analysis. Literature published in the past decade (2009.1–2019.7) were selected and summarized with emphasis on isolation methods of EVs and MS analysis strategies, with the aim to give an overview of MS-based EV proteomic studies and provide a reference for future research. [ABSTRACT FROM AUTHOR]

Composite nanoparticles were used in solid phase micro membrane tip extraction and capillary electrophoresis to determine phenol and p-amino-phenol in wastewater. The optimized conditions were 100 g/L concentration, 40 min contact time, 11 pH, 5 mg/mL nanoparticles amounts, 60 min desorption time, 9 desorption pH and 298 K temperature. Capillary electrophoresis conditions were phosphate buffer (15 mM, pH 7.0) background electrolyte, 18 kV applied voltage, 214 nm UV detection, 30 s sample loading at 23 ± 1 °C. The maximum percent uptakes of p-amino-phenol and phenol were 80.0 and 85.0%. High ratio recoveries of p-amino-phenol and phenol from nanomaterial were 99.0 and 98. Consequently, the actual extractions of p-amino-phenol and phenol from wastewater were 79.2 and 83.30 percent. The migration times of phenol and p-amino-phenol and were 9.0 and 12.0 min. The detection limits of phenol and p-amino-phenols were 0.1 and 0.2 µg/L after extraction and CE. Therefore, this combination of solid phase micro membrane tip extraction and capillary electrophoresis may be considered as the ideal one for monitoring of toxic phenol and p-amino-phenol in water sample. [ABSTRACT FROM AUTHOR]

Multiclass screening of drugs with high resolution mass spectrometry is of great interest due to its high time-efficiency and excellent accuracy. A high-scale, fast screening method for pesticides in fishery drugs was established based on ultrahigh performance liquid chromatography tandem quadrupole-Orbitrap high-resolution mass spectrometer. The target compounds - were diluted in methanol and extracted by ultrasonic treatment, and the extracts were diluted with MeOH-water (1:1, v/v) and centrifuged to remove impurities. The chromatographic separation was performed on an Accucore aQ-MS column (100 mm × 2.1 mm, 2.6 μm) with gradient elution using 0.1% formic acid in water (containing 5 mmol/L ammonium formate) and 0.1% formic acid in methanol (containing 5 mmol/L ammonium formate) in Full Scan/dd-MS2 (TopN) scan mode. A screening database, including mass spectrometric and chromatographic information, was established for identification of compounds. The screening detection limits of methods ranged between 1–500 mg/kg, the recoveries of real samples spiked with the concentration of 10 mg/kg and 100 mg/kg standard mixture ranged from 70% to 110% for more than sixty compounds, and the relative standard deviations (RSDs) were less than 20%. The application of this method showed that target pesticides were screened out in 10 samples out of 21 practical samples, in which the banned pesticide chlorpyrifos were detected in 3 out of the 10 samples. [ABSTRACT FROM AUTHOR]

Ginseng (Panax ginseng) has long been used as a traditional medicine for the prevention and treatment of various diseases. Generally, the harvest time and age of ginseng have been regarded as important factors determining the efficacy of ginseng. However, most studies have mainly focused on the root of ginseng, while studies on other parts of ginseng such as its berry have been relatively limited. Thus, the aim of this study iss to determine effects of harvest time on yields, phenolics/ginsenosides contents, and the antioxidant/anti-elastase activities of ethanol extracts of three- and four-year-old ginseng berry. In both three- and fourfour-year-old ginseng berry extracts, antioxidant and anti-elastase activities tended to increase as berries ripen from the first week to the last week of July. Liquid chromatography-tandem mass spectrometry analysis has revealed that contents of ginsenosides except Rg1 tend to be the highest in fourfour-year-old ginseng berries harvested in early July. These results indicate that biological activities and ginsenoside profiles of ginseng berry extracts depend on their age and harvest time in July, suggesting the importance of harvest time in the development of functional foods and medicinal products containing ginseng berry extracts. To the best of our knowledge, this is the first report on the influence of harvest time on the biological activity and ginsenoside contents of ginseng berry extracts. [ABSTRACT FROM AUTHOR]

In this work, the synthesis, characterization, and application of novel parabens imprinted polymers as highly selective solid-phase extraction (SPE) sorbents have been reported. The imprinted polymers were created using sol–gel molecular imprinting process. All the seven parabens were considered herein in order to check the phase selectivity. By means of a validated HPLC-photodiode array detector (PDA) method all seven parabens were resolved in a single chromatographic run of 25 min. These SPE sorbents, in-house packed in SPE empty cartridges, were first characterized in terms of extraction capability, breakthrough volume, retention volume, hold-up volume, number of theoretical plates, and retention factor. Finally, the device was applied to a real urine sample to check the method feasibility on a very complex matrix. The new paraben imprinted SPE sorbents, not yet present in the literature, potentially encourage the development of novel molecularly imprinted polymers (MIPs) to enhance the extraction efficiency, and consequently the overall analytical performances, when the trace quantification is required. [ABSTRACT FROM AUTHOR]

So far, there is no report on the quality evaluation of lemonade available in the market. In this study, a sample preparation method was developed for the determination of flavonoid glycosides by ultra-performance liquid chromatography–mass spectrometry (UPLC-MS) based on vortex-assisted dispersive liquid-liquid microextraction. First, potential flavonoids in lemonade were scanned and identified by ultra-performance liquid chromatography–time of flight mass spectrometry (UPLC-TOF/MS). Five flavonoid glycosides were identified as eriocitrin, narirutin, hesperidin, rutin, and diosmin according to the molecular formula provided by TOF/MS and subsequent confirmation of the authentic standard. Then, an ultra-performance liquid chromatography–triple quadrupole mass spectrometry (UPLC-QqQ/MS) method was developed to determine these five flavonoid glycosides in lemonade. The results showed that the content of rutin in some lemonade was unreasonably high. We suspected that many illegal manufacturers achieved the goal of low-cost counterfeiting lemonade by adding rutin. This suggested that it was necessary for relevant departments of the state to make stricter regulations on the quality standards of lemonade beverages. [ABSTRACT FROM AUTHOR]

In recent years, heavy metals (HMs) levels in soil and vegetation have increased considerably due to traffic pollution. These pollutants can be taken up from the soil through the root system. The ability of plants to accumulate HMs into their tissues can therefore be used to monitor soil pollution. The aim of this study was to test the ruderal species Senecio vulgaris L., Polygonum aviculare L., and Poa annua L., as possible candidates for biomonitoring Cu, Zn, Cd, Cr, Ni and Pb in multiple environments. The soils analyzed in this work came from three different environments (urban, woodland, and ultramafic), and therefore deeply differed for their metal content, texture, pH, and organic matter (OM) content. All urban soils were characterized by high OM content and presence of anthropogenic metals like Pb, Zn, Cd, and Cu. Woodland soils were sandy and characterized by low metal content and low OM content, and ultramafic soils had high Ni and Cr content. This soil variability affected the bioindication properties of the three studied species, leading to the exclusion of most metals (Zn, Cu, Cr, Cd, and Pb) and one species (P. aviculare) due to the lack of linear relations between metal in soil and metal in plants. Senecio vulgaris and Poa annua, conversely, appeared to be good indicators of Ni in all the soils tested. A high linear correlation between total Ni in soil and Ni concentration in P. annua shoots (R2 = 0.78) was found and similar results were achieved for S. vulgaris (R2 = 0.88). [ABSTRACT FROM AUTHOR]

Saffron is one of the most adulterated food products all over the world because of its high market prize. Therefore, a non-targeted approach based on the combination of headspace flash gas-chromatography with flame ionization detection (HS-GC-FID) and chemometrics was tested and evaluated to check adulteration of this spice with two of the principal plant-derived adulterants: turmeric (Curcuma longa L.) and marigold (Calendula officinalis L.). Chemometric models were carried out through both linear discriminant analysis (LDA) and partial least squares discriminant analysis (PLS-DA) from the gas-chromatographic data. These models were also validated by cross validation (CV) and external validation, which were performed by testing both models on pure spices and artificial mixtures capable of simulating adulterations of saffron with the two adulterants examined. These models gave back satisfactory results. Indeed, both models showed functional internal and external prediction ability. The achieved results point out that the method based on a combination of chemometrics with gas-chromatography may provide a rapid and low-cost screening method for the authentication of saffron. [ABSTRACT FROM AUTHOR]

In this work, the electrochemical behavior of hydrochlorothiazide and pyridoxine on the ethylenediamine-modified glassy carbon electrode were investigated by differential pulse voltammetry. In pH 3.4 Britton-Robinson (B-R) buffer solution, both hydrochlorothiazide and pyridoxine had a pair of sensitive irreversible oxidation peaks, that overlapped in the 1.10 V to 1.20 V potential range. Under the optimum experimental conditions, the peak current was linearly related to hydrochlorothiazide and pyridoxine in the concentration range of 0.10–2.0 μg/mL and 0.02–0.40 μg/mL, respectively. Chemometrics methods, including classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS), were introduced to resolve the overlapped signals and determine the two components in mixtures, which avoided the troublesome steps of separation and purification. Finally, the simultaneous determination of the two components in commercial pharmaceuticals was performed with satisfactory results. [ABSTRACT FROM AUTHOR]

Sporotrichosis occurs worldwide and is caused by the fungus Sporothrix brasiliensis. This agent has a high zoonotic potential and is transmitted mainly by bites and scratches from infected felines. A new association between the drugs clotrimazole and itraconazole is shown to be effective against S. brasiliensis yeasts. This association was formulated as a microemulsion containing benzyl alcohol as oil, Tween® 60 and propylene glycol as surfactant and cosurfactant, respectively, and water. Initially, the compatibility between clotrimazole and itraconazole was studied using differential scanning calorimetry (DSC), thermogravimetric analysis (TG), Fourier transform infrared spectroscopy (FTIR), and X-ray powder diffraction (PXRD). Additionally, a simple and efficient analytical HPLC method was developed to simultaneously determine the concentration of clotrimazole and itraconazole in the novel microemulsion. The developed method proved to be efficient, robust, and reproducible for both components of the microemulsion. We also performed an accelerated stability study of this formulation, and the developed analytical method was applied to monitor the content of active ingredients. Interestingly, these investigations led to the detection of a known clotrimazole degradation product whose structure was confirmed using NMR and HRMS, as well as a possible interaction between itraconazole and benzyl alcohol. [ABSTRACT FROM AUTHOR]

Background: Solasodine is a major bioactive ingredient in Solanum nigrum L. that has strong pharmacological characteristics. Therefore, the development of a simple and effective extraction method for obtaining solasodine is highly important. This study aims to provide a rapid and effective method for extracting solasodine from Solanum nigrum L. by microwave-assisted aqueous two-phase extraction (MAATPE). Methods: First, the high-performance liquid chromatography (HPLC) conditions were established for the detection of solasodine. Then, the aqueous two-phase system (ATPS) compositions were examined. On the basis of the results of single-factor experiments, for a better yield, response surface methodology (RSM) was used to optimize influential factors including the extraction temperature, extraction time and liquid-to-solid ratio. Results: The maximum extraction yield of 7.11 ± 0.08 mg/g was obtained at 44 °C, an extraction time of 15 min, and a liquid-to-solid ratio of 42:1 mL/g in the ATPS consisting of EtOH solvent, (NH4)2SO4, and water (28:16:56, w/w/w). The extraction yield of the alkaloid obtained using this method was markedly higher than those of microwave-assisted extraction (MAE) and ultrasonic-assisted extraction (UAE). Conclusions: In this work, solasodine was extracted by MAATPE for the first time and a high yield was obtained. MAATPE is a simple, rapid, and green technique for extraction from medical plants. Thus, the present study will enable the development of a feasible extraction method of active alkaloids from Solanum nigrum L. [ABSTRACT FROM AUTHOR]

Kanamycin is an aminoglycoside antibiotic widely used in treating animal diseases caused by Gram-negative and Gram-positive infections. Kanamycin has a relatively narrow therapeutic index, and can accumulate in the human body through the food chain. The abuse of kanamycin can have serious side-effects. Therefore, it was necessary to develop a sensitive and selective analysis method to detect kanamycin residue in food to ensure public health. There are many analytical methods to determine kanamycin concentration, among which high performance liquid chromatography (HPLC) is a common and practical tool. This paper presents a review of the application of HPLC analysis of kanamycin in different sample matrices. The different detectors coupled with HPLC, including Ultraviolet (UV)/Fluorescence, Evaporative Light Scattering Detector (ELSD)/Pulsed Electrochemical Detection (PED), and Mass Spectrometry, are discussed. Meanwhile, the strengths and weaknesses of each method are compared. The pre-treatment methods of food samples, including protein precipitation, liquid-liquid extraction (LLE), and solid-phase extraction (SPE) are also summarized in this paper. [ABSTRACT FROM AUTHOR]

Gastrodia elata (G. elata) tuber is a valuable herbal medicine used to treat many diseases. The procedure of establishing a reasonable and feasible quality assessment method for G. elata tuber is important to ensure its clinical safety and efficacy. In this research, an effective and comprehensive evaluation method for assessing the quality of G. elata has been developed, based on the analysis of high performance liquid chromatography (HPLC) fingerprint, combined with the quantitative analysis of multi-components by single marker (QAMS) method. The contents of the seven components, including gastrodin, p-hydroxybenzyl alcohol, p-hydroxy benzaldehyde, parishin A, parishin B, parishin C, and parishin E were determined, simultaneously, using gastrodin as the reference standard. The results demonstrated that there was no significant difference between the QAMS method and the traditional external standard method (ESM) (p > 0.05, RSD < 4.79%), suggesting that QAMS was a reliable and convenient method for the content determination of multiple components, especially when there is a shortage of reference substances. In conclusion, this strategy could be beneficial for simplifying the processes in the quality control of G. elata tuber and giving references to promote the quality standards of herbal medicines. [ABSTRACT FROM AUTHOR]