Ultra-performance Liquid Chromatography Photodiode Research Articles

First analytical confirmation of drug-induced crystal nephropathy in felines caused by GS-441524, the active metabolite of Remdesivir

GS-441524 is an adenosine nucleoside antiviral demonstrating significant efficacy in the treatment of feline infectious peritonitis (FIP), an otherwise fatal illness, resulting from infection with feline coronavirus. However, following the emergence of COVID-19, veterinary development was halted, and Gilead pursued clinical development of a GS-441524 pro-drug, resulting in the approval of Remdesivir under an FDA emergency use authorization. Despite lack of regulatory approval, GS-441524 is available without a prescription through various unlicensed online distributors and is commonly purchased by pet owners for the treatment of FIP. Herein, we report data obtained from the analytical characterization of two feline renal calculi, demonstrating the propensity for GS-441524 to cause renal toxicity through drug-induced crystal nephropathy in vivo. As definitive diagnosis of drug-induced crystal nephropathy requires confirmation of the lithogenic material to accurately attribute a mechanism of toxicity, renal stone composition and crystalline matrix were characterized using ultra-performance liquid chromatography photodiode array detection (UPLC-PDA), ultra-performance liquid chromatography mass spectrometry (LCMS), nuclear magnetic resonance (NMR) spectroscopy, X-ray powder diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR). This work serves to provide the first analytical confirmation of GS-441524-induced crystal nephropathy in an effort to support toxicologic identification of adverse renal effects caused by administration of GS-441524 or any pro-drug thereof.

UPLC-PDA Approach for Simultaneous Quantification of Elvitegravir, Tenofovir, Emtricitabine and Cobicistat in Tablets: An MS-ESI Study for Degradation Products.

A simultaneous ultra-performance liquid chromatography photodiode array detection method was developed and validated for Elvitegravir, Tenofovir and Emtricitabine and Cobicistat drugs in tablet dosage forms. Effective liquid chromatographic quantification was achieved using a Luna C18 (100 × 2.6mm, 1.6μ) column with an acetonitrile: 0.1% v/v trifluoro acetic acid (80:20% v/v) mobile phase and a photo diode array detector at 260nm for a shorter run time of 3min. The respective retention times for Elvitegravir, Tenofovir, Emtricitabine and Cobicistat were 0.311, 0.792, 1.379 and 2.045min. The range of linearity was 37.50-225.00, 2.50-15.00, 50.00-300.00and 37.50-225.00μg/mL for Elvitegravir, Tenofovir, Emtricitabine and Cobicistat, respectively. A mass spectrometer was employed for quantitative analysis using electron spray ionization multiple reaction monitoring in positive mode. The developed method was validated for different parameters to meet the acceptance criteria as per ICH Q2 (R1) guidelines. Using UPLC-ESI-MS, 12 degradants were identified and their mechanisms were studied.

A Fast and Robust Analytical Method Based on QuEChERS Technique using UPLC- PDA for Quantification of Carcinogenic Arylamines in Consumer Goods inclusive of Leather

Arylamines present in leather and textile products are reduced in vivo by cleavage of azo groups to form highly mutagenic and carcinogenic products that pose consumer’s health risk. The major textile and leather products that are offered to consumers need to be safe. In order to ensure safety as per the global regulations, the allowed limit of carcinogenic amines in textile and leather products cannot be more than 20 mg/kg. There are several methods that have been used for extracting the azo dyes and analyzing them in textile and leather products. Most of these methods are polluting from high solvent usage, time consuming, laborious, and have lower recovery rates. In the present study QuEChERS method, (dispersive solid phase extraction-dSPE) method was utilized for extraction of carcinogenic arylamines from dyed leather and textile products. The released arylamines are extracted into acetonitrile using QuEChERS salt and analyzed by Ultra Performance Liquid Chromatography-Photo Diode Array (UPLC-PDA). The extracted product was further confirmed by Gas Chromatography-Mass Spectrometer (GC-MS). The method proposed in this study is novel as it eliminates all significant concerns associated with the official ISO-17234-1 &14362-1 test methods, such as use of solvents like tert-butyl methyl ether (MTBE) and the long duration of analysis. The sample preparation time is minimized from 120 min to 20 min. The developed method is easy to adopt with efficient recovery rate of arylamines in comparison to the official ISO method.

Determination of 35 sulfonamides in pork by magnetic molecularly imprinted polymer-based dispersive solid-phase extraction and ultra-performance liquid chromatography photodiode array method.

Sulfonamide residues in foods of animal origin are potential risks to consumer health, so it is very important to inspect them. Among the previously reported instrumental methods, the best method can only be used to determine at most 22 sulfonamides. Thus, an instrumental method capable of determining more sulfonamide species is desirable. In this study, sulfadoxine was used as a template to synthesize a type of magnetic molecularly imprinted polymer that could recognize 35 sulfonamides. After characterization, this composite was used to develop a dispersive solid-phase extraction method for extraction and purification of the 35 sulfonamides in pork, followed by determination using an ultra-performance liquid chromatography photodiode array method. This composite exhibited high adsorption capacity (11.01-19.21 μg mg-1 ) and high recovery (>89.01%), and could be reused at least ten times. Due to the enrichment effect during sample preparation (enrichment factor 22-66), the limits of detection for determination of the 35 drugs in pork were in the range of 0.08-0.53 ng g-1 . The detection results for some real pork samples were consistent with a liquid chromatographic-tandem mass spectrometric method. After comparison, the present method showed generally better performances than the previously reported sample preparation methods and instrumental methods for detection of sulfonamides. The method developed in the present study could be used as a practical tool for routine detection of sulfonamide residues in pork samples. © 2022 Society of Chemical Industry.

Phenotypic diversity and capsaicinoid content of chilli pepper landraces (Capsicum spp.) from the Yucatan Peninsula

AbstractMexico has a wealth of plant genetic resources, including Capsicum species. In southern Mexico, specifically in the western part of the Yucatan Peninsula, Maya farmers have preserved a great diversity of chilli pepper landraces of C. annuum, C. frutescens and C. chinense. However, the morphological diversity, capsaicinoid content, conservation status and potential use of these species have not been studied. To fill this gap and generate information to support the conservation and use of these species, we characterized the phenotypic diversity and capsaicinoid content for nine chilli pepper landraces from the western Yucatan Peninsula by assessing 15 quantitative and 39 qualitative traits for 10 plants of each landrace. For quantitative variables, two groups of chilli pepper landraces were obtained by principal component analysis and cluster analysis. Group I was formed by Rosita, Bobo, Dulce, Xcat'ik1, Xcat'ik2 and Verde landraces; Group II included the Maax, Bolita and Pico Paloma landraces. For qualitative variables, three groups of chilli pepper landraces were obtained; Group I included Dulce, Bobo, Xcat'ik1, Xcat'ik2 and Verde landraces, Group II only included the Rosita landrace, and Group III included Maax, Bolita and Pico Paloma landraces. Ultra-performance liquid chromatography–photodiode array (UPLC-PDA) quantification of capsaicinoids indicated higher values in landraces Rosita (14,062.3 μg/g D.W), Bolita (5928.1 μg/g D.W), Maax (3438.4 μg/g D.W) and Pico Paloma (3138.9 μg/g D.W). The Yucatan chilli pepper landraces provide valuable diverse germplasm for morphological characteristics and capsaicinoid content that can be used in breeding and conservation programmes.

Phenolic compounds in olive oil by solid phase extraction – Ultra performance liquid chromatography – Photodiode array detection for varietal characterization

An new method for the extraction of phenolic compounds from olive oil has been proposed before the chromatographic analysis by UPLC-PDA (Ultra-Performance Liquid Chromatography-PhotoDiode Array). Recoveries for 20 individual phenolic compounds were compared using three cartridges of solid-phase extraction including C-18, Diol, and DVB (DiVinylBenzene) based cartridges. Diol based cartridge produced the best retention efficiency. The optimized method uses a reduced amount of solvents and allows for the determination of most phenolics in oil samples in less than 10 min. A full discrimination among the most common olive oil varieties was achieved using the relative levels for specific phenolics in the sample. Therefore, based in this study, a fingerprint based on the relative levels for quercetin, luteolin, oleuropein and vanillic acid can be proposed to characterized varietal olive oils. In that way, a detailed composition about phenolic compounds of varietal olive oils would not be needed for discrimination purposes.

Evaluation of Moist Beef Jerkys (dendeng lambok) Nutrition as a Specific-Spiced Traditional Food at West Sumatera, Indonesia

Moist beef jerky (dendeng lambok) is one of traditional food in Indonesia that potential to be introduced to the world. This kind of food is a form of diversification of processed beef products that use natural spices as ingredients that can improve the taste and nutritional value of beef. In this study, the nutritional changes of the beef on the production of moist beef jerky as a specific-spiced traditional food at West Sumatera, Indonesia were evaluated. The production of traditional moist beef jerky that treated with some specific spices prior to frying, might induced the nutritional compound of the raw beef therefore the nutritional properties such as proximate contents, amino acids, fatty acids and in-vitro protein digestibility of the raw beef was compared with the spiced-fried beef. The Association of Official Analytical Chemist’s method, Ultra Performance Liquid Chromatography-Photo Diode Array Detection, Gas Chromatography-Flame ionization Detection and in-vitro enzymatic analysis were used to analyze proximate contents, amino acids, fatty acids and in-vitro protein digestibility of the samples respectively. As the result, the moisture content and carbohydrate content of fried beef decreased significantly compared to the raw beef while the protein and fat content increased. Moreover, the frying process of spiced beef could increased the amino acids, fatty acids and in-vitro protein digestibility of the beef. The present study showed that the quality characteristics of moist beef jerky were significantly improved compared to the raw beef especially on protein profile, fat profile and in-vitro protein digestibility. The utilization of specific spices and frying process on the production of moist beef jerky not only contribute to nutritional properties, but also contribute to its taste and flavor. The increment of amino acids and fatty acids might contribute to the emergence of specific aroma and flavor of produced moist beef jerky. Moreover, the specific study on the interaction of moist beef jerky’s spices on its nutritional properties should be clarified further.

Characterization of Bioactive Compounds of Opuntia ficus-indica (L.) Mill. Seeds from Spanish Cultivars.

Opuntia ficus-indica (L.) Mill. is the Cactaceae plant with the greatest economic relevance in the world. It can be used for medicinal purposes, animal nutrition, production of biofuels and phytoremediation of soils. Due to its high content of bioactive compounds, the prickly pear has antioxidant, antimicrobial and anticancer properties. The aim of this study was to determine the polyphenolic, fatty acid and amino acid profile and characterize the antioxidant capacity of seeds of seven Spanish prickly pear cultivars. A total of 21 metabolites, mainly phenolic acids and flavonols, were identified using ultraperformance liquid chromatography photodiode detector quadrupole/time-of-flight mass spectrometry (UPLC-PDA-Q/TOF-MS). Significant differences were found in the phenolic concentrations of the investigated varieties. The highest amount of phenolic compounds (266.67 mg/kg dry matter) were found in the “Nopal espinoso” variety, while the “Fresa” variety was characterized by the lowest content (34.07 mg/kg DM) of these compounds. In vitro antioxidant capacity was positively correlated with the amount of polyphenols. The amino acid composition of protein contained in prickly pear seeds was influenced by the variety. Glutamic acid was the predominant amino acid followed by arginine, aspartic acid and leucine, independent of prickly pear variety. Overall, 13 different fatty acids were identified and assessed in prickly pear seeds. The dominant fatty acid was linoleic acid, with content varying between 57.72% “Nopal ovalado” and 63.11% “Nopal espinoso”.

Determination of Nitrofuran Metabolites in Fish by Ultraperformance Liquid Chromatography-Photodiode Array Detection with Thermostatic Ultrasound-Assisted Derivatization.

Nitrofuran (NF) is a class of broad-spectrum antibiotics that are used illegally in animal feeding. NF and its metabolites have proven to pose potential risk to human health. To address the current analytical needs to quantify low levels of NF metabolites in animal foods, a sensitive method was developed for simultaneous detection of four NF metabolites in fish products by an ultraperformance liquid chromatography-diode array detector (UPLC-DAD). With 2-nitrobenzaldehyde (2-NBA) as the derivatizing reagent, the metabolites were hydrolyzed and derivatized under the assistance of thermostatic ultrasound. Compared with the current detection methods, the time of the derivatization reaction has been shortened from 16 to 2 h. The relative coefficient of four NF metabolite derivatives reached more than 0.998, with excellent linear relationship. The limits of detection (LODs) and limits of quantification (LOQs) of six repeated determinations reached 0.25–0.33 and 0.80–1.10 μg/kg, respectively. For all four NF metabolites, the limit of detection of the method was below the minimum required performance limit (MRPL) of 1.0 μg/kg, which makes it compatible with the EU requirements. The recoveries ranging from 89.8 to 101.9% with relative standard deviation below 6.5% were obtained for all of the NF metabolites. What’s more, this method was successfully applied for the determination of four NF metabolites in the fish products. As a promising approach, this method could also be extended for the quantitation of NF metabolites in aquaculture and poultry products.

The flavonoid-enriched extract from the root of Smilax china L. inhibits inflammatory responses via the TLR-4-mediated signaling pathway

Ethnopharmacological relevanceSmilax china L. has been used clinically to treat various inflammatory disorders with a long history. Aim of the studyTo investigate the mechanisms underlying anti-inflammatory action of the extract from the herb. Materials and methodsThe extract was identified and quantified using the Ultra Performance Liquid Chromatography-Photo Diode Array-Mass Spectrometer method. The anti-inflammatory activities were examined in xylene-induced mouse ear edema and cotton ball-induced rat granuloma. The inflammatory mediators, pro-inflammatory cytokines and TLR-4-mediated signals in LPS-stimulated RAW264.7 macrophages were determined using ELISA, real-time PCR, Western blot and/or immunofluorescence, respectively. ResultsThe extract was found to enrich flavonoids (44.3%, mainly astilbin, engeletin, isoastilbin, cinchonain Ia, quercetin-3-O-a-L-rhamnopyranoside and chlorogenic acid). The flavonoid-enriched extract (FEE) inhibited xylene-induced mouse ear edema and cotton ball-induced rat granuloma, and suppressed LPS-induced over-release and/or overexpression of tumor necrosis factor-α, cyclooxygenase-2, inducible nitric oxide synthase, interleukin-1β and interleukin-6 in RAW264.7 macrophages. Mechanistically, FEE suppressed protein overexpression of TLR-4 and its downstream signals, MyD88 protein, phosphorylated inhibitory κB-α, NF-κB-P65 and MAPK p38, as well as phosphorylation of phosphoinositide 3-kinase (PI3K) p85α at Tyr607 and Akt at Ser473 in LPS-stimulated macrophages. The mode of the anti-inflammatory action of FEE was similar to that of TAK-242 (a selective TLR-4 inhibitor). ConclusionsThe present results demonstrate that FEE inhibit inflammatory responses via the TLR-4-mediated signaling pathway. Our findings go a new insight into the mechanisms underlying anti-inflammatory action of the herb, and provide a better understanding of its use for inflammatory diseases.

Polyphenol Compounds and Biological Activity of Caper (Capparis spinosa L.) Flowers Buds.

The aim of the study was to analyze potential health-promoting components of caper flower buds (Capparis spinosa L.) at six stages of development in two cultivars. Polyphenol compounds (flavonols, hydroxycinnamic acids, flavan-3-ols) were identified by Liquid Chromatography– quadrupole Time–of–Flight –Mass Spectrofotometer/Mass Spectrofotometer (LC-qTOF-MS/MS) and quantified by Ultra Performance Liquid Chromatography–Photodiode Array-Fluorescence Detector (UPLC-PDA-FL). Moreover, antioxidant properties (ABTS+•, FRAP, and ORAC), anti-diabetic potential (α-amylase and α-glucosidase), and anti-aging activity (acetylcholinesterase (AChE) and butyrylcholinesterase (BuChE)) of the buds were examined. Total phenolic compounds in the investigated caper varied from 10,720 to 3256 mg/100 g dry weight (DW), and depended on a genotype and growing stage of caper flowers. Among six different growing stages, the one named ‘nonpareilles’ was characterized by significantly higher content of polyphenols than the remaining five stages. The flavonols in caper flowers represented a mixture of different glycosylated quercetin, kaempferol, myricetin, and isorhamnetin derivatives, accounting for 38%–67%, 15%–36%, 4%–7%, and 0.8%–3%, respectively, of total flavonols,. Their contents strongly depended on the growth stage. ‘Nonpareilles’ and ‘surfines’ were richer in flavonols than ‘fines’ and ‘gruesas’. Of the six investigated growth stages, ‘nonpareilles’ accumulated the greatest amounts of bioactive compounds that correlated with antioxidant and anti-diabetic properties, and were more potent BuChE than AChE inhibitors.

Effect of Different Yeast Strains and Temperature of Fermentation on Basic Enological Parameters, Polyphenols and Volatile Compounds of Aurore White Wine.

The aim of this study was to investigate the content of phenolics by Ultra Performance Liquid Chromatography–Photodiode Array (UPLC–PDA), and volatile compounds by Gas Chromatography–Mass Spectroscopy (GC–MS), antioxidant capacity by 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) radical cation (ABTS•+) and ferric-reducing antioxidant power (FRAP) assay, and color of Comission Internationale de l’Eclairage system (CIE) L*a*b* cv. Aurora white wine depending on fermentation conditions (a temperature of 12 °C vs. 20 °C and type of natural and commercial yeast (Saccharomyces cerevisiae vs. Saccharomyces bayanus)). The final wine differed in the content of total phenolic compounds (201.0–287.2 mg/L), except for the variants fermented at 20 °C with S. cerevisiae (321.9 and 329.4 mg/L for S. cerevisiae as Challenge Aroma White and SIHA® Cryaroma type, respectively). A decrease in antioxidant activity ranging from 43.3% to 65.4% (ABTS and FRAP assay) in the matured wine vs. must was demonstrated. S. cerevisiae wine was also characterized by the highest content of total volatile compounds (3.7–4.2 mg/L vs. 1.3 mg/L in the must). In general, the wine obtained with S. cerevisiae had higher alcohol content, antioxidant capacity, and was richer in polyphenolic and volatile compounds.

Pharmacokinetics of meropenem in burn patients with infections caused by Gram-negative bacteria: Are we getting close to the right treatment?

Infections caused by multidrug-resistant Gram-negative bacteria are associated with high mortality. A relevant concern is the efficacy of antibiotic therapy in burn patients in whom pathophysiological changes strongly influence pharmacokinetic (PK) parameters. This study aimed to describe the PK parameters of meropenem in a population of burn patients. Blood samples were collected immediately before and 2 h and 5 h after the start of intravenous drug administration. Plasma meropenem concentrations were determined using an ultra-performance liquid chromatography-photodiode array method. Seventeen burn patients were enrolled in the study. Thirteen patients (76%) were treated with meropenem for infections byPseudomonas aeruginosa or Acinetobacter baumannii isolated from blood or wounds. Mean Cmax, Cmin, AUC0-24, half-life, drug clearance and volume of distribution were 28.9 mg/L, 3.7 mg/L, 280.2 mg h/L, 2.0 h, 19.0 L/h and 44.4 L, respectively. Six patients (35%) achieved a Cmin ≥3.3 mg/L and seven patients (41%) achieved a Cmax ≥ 28.4 mg/L, whilst nine patients (53%) achieved an AUC0-24 of >226 mg h/L. Given a minimum inhibitory concentration (MIC) of 0.5 mg/L, all patients satisfied the target AUC/MIC of >125, but when the MIC rises to 2 mg/L (the ECOFF), only five patients reached the desired AUC/MIC. Regarding fT>MIC at an MIC of 2 mg/L with a 2-h infusion time, 13 patients (76%) achieved the PK target (>75%). These data suggest that a combined 2-h infusion with a higher dosage of meropenem, including a loading dose, may be successful to achieve effective PK parameters.

Profile of Bioactive Compounds in the Morphological Parts of Wild Fallopia japonica (Houtt) and Fallopia sachalinensis (F. Schmidt) and Their Antioxidative Activity.

The aim of this study was to determine the content of triterpenoids and polyphenols, and antioxidative activity in leaves, stalks, and roots of plants from the species Fallopia as well as to present the main relationship between them. Polyphenolic compounds and triterpenoids were identified with liquid chromatography-photodiode detector-mass spectrometry/quadrupole time of flight (LC-MS-Q/TOF; qualitatively) and quantified with an ultra-performance liquid chromatography-photodiode detector (UPLC-PDA (quantitatively), and their antioxidative activity was determined with radical scavenging capacity (ABTS) and oxygen radical absorbance capacity (ORAC) assays. Generally, the wild Fallopia japonica Houtt. species had 1.2 times higher content of bioactive compounds and antioxidative activity than Fallopia sachalinensis. Contents of polyphenolic compounds determined in leaves, stalks, and roots were on average 17.81, 10.60, and 9.02 g/100 g of dry weight (DW), whereas the average contents of triterpenoids reached 0.78, 0.70, and 0.50 g/100 g DW, respectively. The leaves were a better source of polymeric procyanidins, phenolic acids, flavones, and flavonols, as well as oleanolic and ursolic acids than the other morphological parts of the tested plants. However, the roots were an excellent source of flavan-3-ols (monomeric and oligomer) and stilbenes, such as resveratrol, and their derivatives. The results obtained showed significant differences between plants of the wild Fallopia species and their morphological parts, and enabled selecting the most valuable morphological part of the tested plants to be used for food enrichment and nutraceuticals production. Therefore, the leaves seem to be the best as potential food additives for health, due to the above-average content of polyphenolic compounds and triterpenoids. In turn, roots, with their high contents of stilbenes and polyphenolic compounds, represent a good material for the medical, pharmaceutical, and cosmetic industries. The principal component analysis of the plants of wild Fallopia species and their morphological parts confirmed significant differences in their chemical composition.

Antidiabetic, Anticholinesterase and Antioxidant Activity vs. Terpenoids and Phenolic Compounds in Selected New Cultivars and Hybrids of Artichoke Cynara scolymus L.

The aim of the study was to analyze the chemical composition of new artichoke cultivars and hybrids and to assess their potential health-promoting properties. Polyphenols, carotenoids and chlorophylls were identified by liquid chromatography-photodiode detector-mass spectrometry/quadrupole time of flight (LC-PDA-MS/QTof) and quantified by ultra performance liquid chromatography-photodiode detector (UPLC-PDA). Sugar and organic acid profiles were prepared, and antioxidant capacity (ABTS, FRAP and ORAC) and in vitro antidiabetic (inhibition of α-amylase and α-glucosidase) and anticholinesterase (inhibition of acetylcholinesterase (AChE) and butyrylcholinesterase (BuChE)) potentials were evaluated. The analyses revealed a highly varied content of bioactive compounds and great health-promoting potential significantly depending on a cultivar. The content of polyphenolic compounds ranged from 1681.49 (“Sambo”) to 3638.91 (“Symphony”) mg/100 g of dry weight (DW). “Blanca de Tudela” contained the highest amounts of carotenoids and chlorophylls (3761.91 mg/100 g DW) and exhibited high ABTS and ORAC capacity. Inhibition of antidiabetic enzymes was significant in cvs. “Symphony” and “Calico”. Additionally, all tested cultivars and hybrids turned out to be effective inhibitors of neurodegenerative enzymes.

Validation of ultra performance liquid chromatography photodiode array method for determination of mycophenolic acid in human plasma and its application

Validation of ultra performance liquid chromatography photodiode array method for determination of mycophenolic acid in human plasma and its application

UPLC-PDA-Q/TOF-MS identification of bioactive compounds and on-line UPLC-ABTS assay in Fallopia japonica Houtt and Fallopia sachalinensis (F.Schmidt) leaves and rhizomes grown in Poland

The activity of polyphenolic compounds, triterpenoids, carotenoids, chlorophylls and antioxidants in leaves and rhizomes of Fallopia japonica Houtt and Fallopia sachalinensis (F.Schmidt) grown in Poland was investigated. Leaves and rhizomes were assessed for the presence of bioactive compounds with the ultra-performance liquid chromatography photodiode detector-quadrupole/time-of-flight mass spectrometry (UPLC-PDA-Q/TOF-MS) method, and for antioxidant activity with the on-line UPLC-ABTS screening. Forty-six polyphenolic compounds (15 phenolic acids, 12 flavones and flavonols, 11 flavan-3-ols and 8 stilbenes), were identified in Fallopia japonica and Fallopia sachalinensis. Furthermore, accurate mass measurement technique was for the first time in Fallopia japonica Houtt and Fallopia sachalinensis (F.Schmidt) in leaves and rhizomes it identified 25 new compounds belonging to carotenoids (9), chlorophylls (13) and triterpenoids (3) as well as rated the antioxidant properties of each polyphenolic compound. Major qualitative differences were found in the profiles. The leaves and rhizomes were found to be a good source not only of (average 20408.18 and 2716.42 mg/100 g dm), but also chlorophylls (average 179.97 and 43.82 mg/100 g dm), carotenoids (average 100.23 and 53.25 mg/100 g dm) and triterpenoids (average 580.87 and 434.05 mg/100 g dm). The content of bioactive compounds in Fallopia japonica Houtt was around 8.0, 4.0, 2.0 and 1.3 times higher than the content of polyphenols, chlorophylls, carotenoids and triterpenoids in Fallopia sachalinensis (F.Schmidt). The accurate identification of Fallopia bioactive compounds is an indispensable detailed knowledge of the profile and step toward better understanding of the medicinal properties of the species and also potentially more extensive use of the plant.

Spectrochromatographic determination of dorzolamide hydrochloride and timolol maleate in an ophthalmic solution using three-way analysis methods

In this study, the simultaneous spectrochromatographic determination of dorzolamide hydrochloride (DOR) and timolol maleate (TMM) in an ophthalmic formulation was performed by applying multiway resolution methods, parallel factor analysis (PARAFAC) and three way partial least squares (3W-PLS) models. In similar manner, unfolded partial least squares (U-PLS) approach was applied to the UPLC analysis of the related drugs. For the three-way resolutions, the ultra-performance liquid chromatography–photodiode array (UPLC-PDA) data array of the calibration samples and others (validation and commercial samples) containing the analyzed drugs (DOR and TMM) and thiamine hydrochloride as an internal standard (IS) was decomposed into triads or trilinear components. These three different calibration models were employed for the spectrochromatographic resolution of a commercial ophthalmic formulation of DOR and TMM and then successful quantitation results were obtained. Analysis results provided by applying three-way and two-way resolutions were statistically compared to those obtained by the newly developed standard UPLC approach. It was observed that the proposed methods gave comparable determination results for analysis of the DOR-TMM ophthalmic formulation.

Development and Validation of UPLC–PDA Method for Quality Control of Dikamali gum—A Natural Tablet Binder: Fast Simultaneous Quantitation of Six Polymethoxyflavones

Dikamali gum (Gardenia lucida Roxb., Family—Rubiaceae) in wet and dry form is used as one of the popular tablet binders in the Indian traditional herbal formulations. Recently, its application as a binder in modern drug delivery has also been reported. However, its quality specification is yet to be established. To the best of our knowledge, no validated method is reported so far for the quality assurance of Dikamali. A new reverse-phase ultraperformance liquid chromatography–photodiode array (UPLC–PDA) method was developed for the simultaneous quantification of six polymethoxyflavones (PMFs), viz., gardenin E, gardenin D, xanthomicrol, 5-desmethynobiletin, gardenin A, and gardenin B, in Dikamali gum using a Waters X-select C18 (2.5 µm, 2.1 × 100 mm) column. The influence of acid additive in mobile phase on peak response and column temperature on the peak resolution was also investigated. ICH guideline was followed for method validation of analytical procedures for the compliance of precision, accuracy, linearity, etc. The method is about three times faster than classical HPLC analysis and completed within 15 min. The limits of detection (LOD) and limit of quantitation (LOQ) were in the range 0.02–0.06 and 0.08–0.20 µg mL− 1, respectively. Calibration curves were linear from 0.18 to 1.78 µg mL− 1 with acceptable correlation coefficients ranged 0.9993–0.9999. The percent mean recoveries of the PMFs were ranged from 96.07 to 101.69%. Successful analysis of three G. lucida samples from different locations demonstrated the method to be reproducible and convenient. The present work also provides some references for quality specification of G. lucida based on polymethoxyflavones.

Skład chemiczny etanolowego ekstraktu z propolisu i jego aktywność biologiczna wobec grzybów pleśniowych

Introduction. Propolis is a natural material whose extracts indicate numerous biological activities, including antifungal, antibacterial, antioxidant and anticancer. Phenolic compounds (flavonoids as well as phenolic acids and their esters) are one of the most frequently mentioned group of propolis components responsible for the biological activity of propolis extracts. Another group of components identified in propolis is elements, including macro- and microelements as well as heavy metals. Aim. The aim of the study was to determine the biological activity of the ethanolic propolis extract originated form Warmian-Masurian Voivodeship against moulds and to analyze concentration of selected flavonoids and elements present in the extract. Material and methods. The biological activity of the propolis extract obtained from a raw propolis originated from Warmian-Masurian Voivodeship against moulds was determined by dilution in nutrient solution. The content of selected flavonoids (apigenin, pinocembrin, kaempferol and galangin) in the propolis extract was determined using ultra-performance liquid chromatography photodiode array detection tandem mass spectrometric method. The concentration of elements in the propolis extract was analyzed by flame atomic absorption spectrometry. Results. The propolis extract was characterized by activity against all tested fungal strains. It showed the highest activity towards Chaetomium globosum and Penicillium cyclopium. Among analyzed flavonoids, the highest concentration in the propolis extract was determined for pinocembrin. In addition, high concentrations of Na, Mg, K, Ca and Fe were found in the propolis extract, and no toxic heavy metals were found. Conclusions. The ethanolic propolis extract of national origin shows biological activity against tested moulds and it is a valuable source of flavonoids, as well as macro- and microelements.