Pharmacological, toxicological and phytochemical analysis of Spondias dulcis parkinson.

Spondias dulcis Parkinson have been used in traditional medicine in Asia, Oceania, and South America, for different diseases conditions and as a functional food. The scientific literature described as different potential pharmacology such as antioxidant, anti-inflammatory, antimicrobial, thrombolytic and enzymatic inhibitor. This study aimed to: (1) establish the pharmacological activity in intestinal motility in vivo and antioxidant activity in vitro; (2) perform the acute toxicology test in mouse; (3) characterize the phytochemical profile based on counter-current chromatography (CCC) and NMR analysis. The results revealed a laxative effect of S. dulcis extract and a high antioxidant activity (IC50 = 5.10 for DPPH assay and 14.14 for hydrogen peroxide scavenging test). No side effects were observed in the oral acute toxicity test for a dose up to 2000 mg/kg. The chemical profile was identified by CCC and NMR, and the comparison of the data obtained with previous literature revealed the presence of the flavonoid rutin (Quercetin-3-O-rutinoside) in the extract.

A Clean, Sustainable and Stability-Indicating Method for the Quantification of Ceftriaxone Sodium in Pharmaceutical Product by HPLC.

Ceftriaxone sodium is a widely used antimicrobial, which is only available as a lyophilized powder. The presence of methods for evaluating the quality of this product is very important and helps to ensure its effectiveness, in addition to contributing to the fight against bacterial resistance. Therefore, a clean and sustainable high-performance liquid chromatography (HPLC) method has been developed for evaluating ceftriaxone stability in pharmaceutical product. A Zorbax SB C18 (150 × 4.6 mm, 5 µm) column was maintained at 25°C; the mobile phase consisted of purified water acidified with 0.2% orthophosphoric acid and ethanol (87: 13, v/v) at a flow rate of 0.9 mL min-1. The detection wavelength was set at 260 nm. The method was linear over a concentration range of 20-120 µg mL-1, precise with relative standard deviations <2%, robust in the event of minor changes to the original method conditions, accurate with recovery between 98% and 102% and specific to degradation products. The retention time for ceftriaxone sodium was ~4.6 minutes. This work shows an ecologically correct option by HPLC method for the evaluation of ceftriaxone sodium in pharmaceutical product, as well as its stability, which addresses the requirements of the current green and sustainable analytical chemistry.

New and potential properties, characteristics, and analytical methods of ferulic acid: A review

Abstract Phenolic compounds are widely distributed in the plant kingdom and in the microorganisms. Cinnamic acid and its hydroxylated derivative-ferulic acid, are phenolic compounds. Ferulic acid possesses antioxidant potential, as well as anti-cancer, anti-inflammatory, and antimicrobial properties. It prevents the harmful effects of radiation both as an ultraviolet absorber and as a free radical scavenger; it is not cytotoxic. Although ferulic acid has beneficial properties, it is hardly used in cosmetic preparations and has been rarely studied in the literature. Herein, we review the literature on ferulic acid, to provide information which can contribute to further research on the compound.

A New and Ecological Method to Quantify Vancomycin in Pharmaceutical Product by Infrared Spectrometry.

Vancomycin, an antimicrobial, does not present quantitative method by infrared spectrometry in the literature for the evaluation of a pharmaceutical product. This technique is considered a clean alternative because in the main, there is no solvent involved and the generation of waste is reduced. So, the aim of this study was to develop and validate a new, ecological, low cost and fast method by infrared spectrometry using KBr and band between 1450-1375 cm-1. It was linear in the range of 1.0-2.0 mg/150 mg, with a correlation coefficient of 0.9994. Selective when the spectra of vancomycin reference and sample were compared. Precise by repeatability (2.29%) and intermediate precision (3.12%). Accurate with average recovery of 99.37% and robust when strength and compression time of the pellets and KBr brand were varied. Considering all the methods found in literature, there is not one using infrared spectrometry for quantitative purpose, so the method developed and validated could be considered an innovation and clean alternative. This is due to the fact that it is fast, easy to handle, low cost, and non-toxic as well as generating minimal waste. The method can be applied in the routine analysis of vancomycin dosage form and is an important option for the current and sustainable pharmaceutical analysis.

Eco-Friendly Pharmaceutical Analysis of Rifaximin in Tablets by HPLC-MS and Microbiological Turbidimetry.

Rifaximin, an antimicrobial used for the treatment of various diseases, lacks analytical methods in official compendia for evaluation of the final product. This paper presents an eco-friendly protocol for rifaximin tablets by high performance liquid chromatography coupled with mass spectrometry (HPLC-MS). The method was completely validated according to the International Conference on Harmonization guidelines and developed following the concept of Quality by Design. The separation was achieved using a C18 column, purified water +0.1% glacial acetic acid and ethyl alcohol, 52:48 (v/v), as mobile phase, 0.9 mL min-1 at 290 nm and ambient room temperature. Mass spectral analyses were performed using electrospray ionization (ESI) ion source and ion trap mass analyzer. The method was linear over the concentration range of 5-50 µg mL-1. The sample was subjected to acidic, basic, neutral, oxidative and photolytic degradation. Degradation products did not interfere in the quantification of the rifaximin, so the method can be considered indicative of stability. Degradation products were also evaluated individually by microbiological method using Escherichia coli. The validated method could be used promisingly as green analytical strategies for detection and quantification of rifaximin in tablets.

An Ecological and Miniaturized Biological Method for the Analysis of Daptomycin Potency.

BACKGROUND: Physicochemical and microbiological methods are found in the literature for the analysis of daptomycin, an antimicrobial. OBJECTIVE: This paper brings a miniaturized turbidimetric microbiological method for analysis of daptomycin in lyophilized powder. METHODS: The method was performed using 96-well microplates, 4-h incubation, 2, 4 and 8 µg/mL, 7% Staphylococcus aureus ATCC 6538 IAL 2082, and BHI broth. RESULTS: Linearity was proven by obtaining analytical curves with a correlation coefficient greater than 0.99 and statistical evaluation by ANOVA. The method was also selective, since the standard and sample analytical curves were parallel, proving that the excipient does not interfere with daptomycin analysis. Intraday, interday and inter-analyst precision presented RSDs of 2, 2.27, and 1.08%, respectively. Accuracy was assessed by the recovery test, where known quantities of standard solution are added to the sample and an average recovery value of 100.73% (RSD = 0.71%) was obtained. The present method was robust when minor changes were made in the parameters of used antimicrobial volume, inoculum volume and incubation time. CONCLUSIONS: This work is an innovative and ecological proposal and has advantages such as (i) less waste generation, (ii) miniaturized quantities of sample, culture media and inoculum, (iii) no need to use formaldehyde as in the traditional turbidimetric method, (iv) lower volume of glassware used and (v) shorter incubation time compared to other methods as agar diffusion requiring approximately 24 h. HIGHLIGHTS: This work is focuses on a current, innovative and sustainable theme for pharmaceutical analysis around the world.

Miniaturized Microbiological Method to Determine the Potency of Rifaximin in Tablets.

BACKGROUND: Rifaximin, a semi-synthetic antimicrobial, does not present microbiological method described in official compendia, and there is a lack of literature on this topic. The quality control of antimicrobials is extremely important to evaluate the real potency of pharmaceutical products. OBJECTIVE: A miniaturized turbidimetric method for determining the potency of rifaximin in tablets was developed and validated by turbidimetry, according to the international guidelines. METHOD: Escherichia coli ATCC 10536 IAL 2393, brain heart infusion (BHI) broth, inoculum at 8%, rifaximin in purified water with 20% ethanol at 5, 10, and 20 µg/mL and 530 nm were used. RESULTS: The method was considered selective for rifaximin, as the adjuvants did not show activity; linear with correlation coefficients 0.9998 for standard and 0.9999 for sample; accurate with 99.73% recovery; precise with RSD less than 3%; and robust in the face of small variations in (i) rifaximin volume, (ii) proportion of ethanol, (iii) inoculum volume. CONCLUSIONS: The method is considered adequate and safe to evaluate the potency of rifaximin in tablets, contemplating speed, low cost, low waste generation, and ease of operation. HIGHLIGHTS: This work usescurrent, sustainable, and green analytical chemistry and can be used in the routine analyses of rifaximin by laboratories and the pharmaceutical industry around the world.

Cephalothin: Review of Characteristics, Properties, and Status of Analytical Methods.

BACKGROUND: Cephalothin (CET), a first generation cephalosporin, is the most efficient cephalosporin against resistant microorganisms. Many studies found in literature and pharmacopeias propose analytical methods which are most commonly HPLC and microbiological assays. OBJECTIVE: This paper shows a brief review of analytical methods to quantify CET with a green analytical chemistry approach. METHOD: The research data were collected from the literature and official compendia. RESULTS: Most of the analytical methods to determine CET were performed by HPLC and agar diffusion in pharmaceuticals, blood, urine, or water. Other analytical methods were found, such as UV-Vis, iodometry, fluorimetry, IR/Raman, electrochemical, and others in less quantity. One important aspect is that these methods use organic and toxic solvents like methanol and acetonitrile and only about 4% of the methods found use water as solvent. CONCLUSIONS: Research about analytical methods for CET focusing on green analytical chemistry is of great importance and could optimize its analysis in pharmaceutical industries and help to guarantee the quality of the product. More than just the development of new techniques, it is possible to enhance the ones that already exist, applying the green analytical chemistry principles. In this way, it will be possible to reduce the environmental impacts caused by other analytical procedures. HIGHLIGHTS: This work shows a brief review of literature and pharmacopeias of analytical methods to quantify CET. Its quality control can be updated to meet the needs of current analytical chemistry and to fit into sustainable and eco-friendly analysis.

Turbidimetric Method: A Multi-Advantageous Option for Assessing the Potency of Ceftriaxone Sodium in Powder for Injection.

BACKGROUND: Ceftriaxone sodium, an antimicrobial used in parenteral form, does not have a microbiological method by turbidimetry described in the literature. For drugs from antimicrobial class, the existence of a microbiological method for assessing their potency is essential. Not only are the results from the physical-chemical methods enough, but microbiological analyzes are also necessary. OBJECTIVE AND METHODS: Thus, this paper reports the development and validation of an efficient, accurate, reproducible, fast, and low-cost microbiological assay by turbidimetry to quantify ceftriaxone sodium in powder for injection. Water was used as the diluent to prepare the ceftriaxone solutions. BHI broth as used as culture media for the growth of the S. aureus ATCC 6538 at 9%. RESULTS: The method was linear in the range of 100-196 µg/mL, selective against the sample adjuvants and the forced degradation test, precise (intraday RSD 4.53%, interday RSD 3.85% and between analysts tcalculated 0.14 < 2.23 tcritical), accurate with recovery of 100.33% and robust against minor changes in the volume of culture medium used, wavelength, incubation time, and inoculum concentration. CONCLUSIONS AND HIGHLIGHTS: The turbidimetric method developed in this paper is a convenient and valuable alternative to the routine quality control of ceftriaxone sodium in powder for injection, since it allows a reliable quantification and can be used to complement the physical-chemical analysis.

Short-Stability Study of Rifaximin-Based Samples.

BACKGROUND: Rifaximin is an oral antimicrobial with a daily dose ranging from 600 to 800 mg. It is classified as Class IV in the Biopharmaceutic Classification System. Thus, rifaximin-based samples were developed by complexation to ß-cyclodextrin using a phase solubility diagram, and malaxation and decreasing particle size using wet milling. OBJECTIVE: Concomitant to the pharmaceutical technology, a stability studywas undertaken with the objective of verifying the integrity of the drug. METHODS: The stability of the new samples were studied for 6 months, without interruption, under controlled conditions of temperature and humidity in a climatic chamber. They were analyzed simultaneously by HPLC and microbiological turbidimetry at zero, 3, and 6 months. RESULTS: Two of the samples follow second reaction order and one follows zero reaction order. Microbiological analysis proved to be important in assessing the potency of rifaximin in one of the samples, and its results were more consistent than the results by HPLC. CONCLUSIONS: The rifaximin-based samples were stable under controlled temperature and humidity conditions and the physical-chemical and microbiological methods were able to evaluate their behavior during the 6-month study. HIGHLIGHTS: It is worth considering the development of these products, since the design process of formulation and pharmaceutical technology is financially more attractive than the development of new drugs that require high levels of investment in research and development, innovation of public policies, and regulatory actions.

Current Status of Vancomycin Analytical Methods.

BACKGROUND: The glycopeptide antibiotics are a class of antimicrobial drugs that are an important alternative for cases of bacterial infections resistant to penicillins, besides being able to be used to treat infections in people allergic to pencilin. They have great activity against Gram-positive microorganisms, including methicillin-resistant Staphylococcus aureus (MRSA), by inhibiting the cell wall synthesis. OBJECTIVE: There are many analytical methods in the literature for determination of antimicrobial glycopeptide vancomycin in different matrixes that are very effective; however, all of them use toxic solvents, contributing to the generation of waste, causing damage to the environment and to the operator, as well as increased costs of analysis. RESULTS: The most prevailing method found was high performance liquid chromatography (HPLC), followed by microbiological assays and, in less quantity, spectrometric methods. The chromatographic methods use organic solvents that are toxic, such as acetonitrile and methanol, and buffer solutions, that can damage the equipment and the column. In the microbiological assays the disc diffusion methods are still in the majority. The spectrophotometric methods were based in the UV-Vis region using buffer solutions as a diluent. CONCLUSIONS: All these methods can become greener, following green analytical chemistry principles, which could bring benefits both to the environment and the operator, and reduce costs. HIGHLIGHTS: In this paper, a literature review regarding analytical methods for determination of vancomycin was carried out with a suggestion of greener alternatives.

Turbidimetric Method: A New, Ecological, and Fast Way to Evaluate of Vancomycin Potency.

BACKGROUND: Vancomycin, an antimicrobial, has many microbiological methods in literature, but it was not found any that follows the green chemistry principles. OBJECTIVE: The aim of this work was to develop and validate a new microbiological analytical method with a green view to determine the vancomycin potency in lyophilized powder using less quantity of diluents and culture medium, minimizing the costs and reducing the time of analysis. METHODS: The objective will be achieved using the microbiological method by turbidimetry. RESULTS: Water was used as the diluent to prepare the vancomycin solution. BHI broth as used as culture media for the growth of the S. aureus ATCC 25923. The method was linear in the range of 30, 39 and 50.7 µg/mL. It was selective, with vancomycin reference and sample absorbance values very similar. The precision of the method was proved at intraday (RSD 4.42 %), interday (RSD 3.56 %) and intermediate levels (RSD 2.03%). It was accurate with mean recovery of 100.71 % and robust when changes were performed in three parameters of the method and analyzed by the F-Test and t-Test. CONCLUSIONS: The method for evaluating the potency of vancomycin in pharmaceutical product was successfully developed and validated. HIGHLIGHTS: The method can be applied to routine quality control of vancomycin product as an alternative that contemplates the green analytical chemistry and the current pharmaceutical analyzes.

A Review of Analytical Methods for the Determination of Hypericin in Foods, Herbal, Biological and Pharmaceutical Matrices.

AIMS: A review of analytical methods for the determination of hypericin in foods, herbal, biological and pharmaceutical matrices. BACKGROUND: Hypericin (HYP) is a naturally-occurring pigment obtained from some plants of the genus Hypericum. Although HYP has been known for many years, it has recently attracted attention due to its varied biological properties, such as anti-inflammatory and antidepressant activity and it is also an efficient photosensitizer. OBJECTIVE: The objective of this review is to provide insights into the physicochemical properties of HYP, as well as to report the analytical methods existing in the literature and official compendia for different matrices. METHODS: The survey data were collected by Google Scholar® and Scopus® using keys terms. RESULT: Analytical methods involving HYP are mainly concerned with the quality control of pharmaceutical preparations, foods, beverages, biological samples and drug delivery systems using different types of analysis methods. Some difficulties have also been identified due to the physicochemical properties of HYP. It presents great solubility in alkaline solutions, organic bases and common polar organic solvents. CONCLUSION: It can be analyzed by thin layer chromatography, spectrophotometry in the ultraviolet region, but the most commonly used method is by HPLC. HYP presents monographs in the American, British and European Pharmacopoeias, however, the methods of analysis are not yet harmonized.

Miniaturized turbidimetric assay: A green option for the analysis of besifloxacin in ophthalmic suspension.

Besifloxacin is an important antimicrobial agent, belonging to the class of fluoroquinolones, used in the treatment of infectious conjunctivitis. Quality control of this active pharmaceutical ingredient is essential, since poor quality antimicrobials may contribute to the aggravation of the worrying picture of bacterial resistance. Thus, analytical methods need to be developed, validated and improved for that purpose. It is also important that these methods be environmentally friendly, as ensuring the quality of products without harming the environment meets the global needs. The aim of the study was the development and validation of a miniaturized turbidimetric microbiological method for the analysis of besifloxacin hydrochloride (BSF) in ophthalmic suspension. The analyzes were performed in 96-well microplates using Staphylococcus epidermidis ATCC 12228 as test microorganism and BHI broth. The method was validated according to ICH guidelines and showed to be linear (in a range of 0.5-8.0 µg mL-1), precise, accurate, robust and selective. Study of photo-degradation kinetics of BSF sample showed a zero order reaction. A comparative study with a previously validated HPLC method showed that the methods are interchangeable. This work shows the great potential of the proposed method of being introduced in routine analyzes of quality control of BSF in ophthalmic suspension as an option in line with the principles of Green Chemistry.

A critical review of HPLC-based analytical methods for quantification of Linezolid.

Linezolid is a synthetic antimicrobial agent belonging to the oxazolidinone class. Since its approval in the year 2000 until now, linezolid remains the main representative drug for the oxazolidinone class of drugs, which is used in therapy due to its unique mode of action, which involves inhibition of protein synthesis. As linezolid holds great importance in antimicrobial therapy, it is necessary to compile the various analytical methods that have been reported in the literature for its analysis. Analytical techniques used for pharmaceutical analyses and therapeutic drug monitoring play an important role in comprehending the aspects regarding bioavailability, bioequivalence, and therapeutic monitoring during patient follow-ups. Even though linezolid has had the approval for clinical use for more than 18 years now, most of the analytical methods for its determination reported in the scientific literature are the ones which utilize HPLC. Therefore, the present review provides a summary of the HPLC-based methods used in the determination and quantification of linezolid in different matrices since the time of its discovery.

In vitro methods to determine the antioxidant activity of caffeic acid.

Caffeic acid (CA) is a plant metabolite acting as a carcinogenic inhibitor, and exhibits a high antioxidant effect and some antimicrobial activity. Besides, this compound can be useful in the prevention of heart diseases and atherosclerosis, among others. The present study aims to determine the in vitro antioxidant activity of CA in order to increase the frequency of its use and reliability in the prevention of damage caused by free radicals and other reactive species. The tests performed were as follows: Radical anion superoxide capture; crocin bleaching assay; capturing ability of hypochlorous acid; H2O2 capture; capturing capacity of the ABTS•+/DPPH•; and SOD-like activity. The values of the CA antioxidant activity were very close to the values of standards in all tests. Besides, CA presented an antioxidant activity greater than that of ascorbic acid and trolox, and its advantages include higher stability than ascorbic acid and extraction from natural sources, as opposed to trolox.

Eco-friendly Evaluation of Rifaximin in Tablets by Capillary Electrophoresis.

Rifaximin, an oral antimicrobial, has no standardized analytical methods in many official compendia. In this context, the aim was to develop and validate an analytical method by capillary electrophoresis for quantification of rifaximin in tablets. The choice of capillary electrophoresis was based on the concepts of green analytical chemistry, taking into account the health of the operator and environment, analytical conscience, as well as the parameters of linearity, selectivity, precision, accuracy and robustness. The method was linear between 50 and 500 µg mL-1 (r = 0.9993) using purified water and ethanol in the sample preparation, silica capillary, borate buffer 25 mM pH 9.5, 20 kV and 290 nm. It presented good precision intraday (1.30%) and interday (1.56%). The accuracy complied with average recovery of 100.24%, as well as selectivity in the presence of impurities and degradation products and robustness against variations in the concentration, pH, rinse time of the buffer, voltage, wavelength, injection time and temperature. The capillary electrophoresis method developed for the evaluation of rifaximin tablets is low cost, fast, miniaturized, clean and environmentally friendly and can be used by laboratories and chemical and pharmaceutical industries for quality control of the drug.

Application of the Principles of Green Chemistry for the Development of a New and Sensitive Method for Analysis of Ertapenem Sodium by Capillary Electrophoresis.

An innovative method is validated for the analysis of ertapenem sodium by capillary electrophoresis using potassium phosphate buffer 10 mM pH 7 and 15 kV voltage, in the concentration range of 70 to 120 µg mL-1. Ertapenem had a migration time of 3.15 minutes and the linearity curve was y = 2281.7 x - 24495 with a R2 = 0.9994. Thus, we propose a routine analysis method that meets the principles of green analytical chemistry for the routine analysis of ertapenem sodium by capillary electrophoresis.

Submission of Rifaximin to Different Techniques: Characterization, Solubility Study, and Microbiological Evaluation.

Rifaximin, an oral antimicrobial drug, is marketed as 200-mg tablets. The daily dose ranges from 600 mg (1 tablet 3 times a day) to 800 mg (2 tablets twice a day). It is used for a wide range of ages, from adults to children, since it is indicated for the treatment of hepatic encephalopathy, travelers' diarrhea, irritable bowel syndrome, Clostridium difficile, ulcerative colitis, and acute diarrhea. The success of pharmacotherapy will depend on correct fulfillment of drug administration; however, it becomes difficult when the tablets are large and the doses are frequent. Rifaximin belongs to class IV according to the Biopharmaceutic Classification System (BCS), meaning that it is both poorly soluble and poorly permeable. Thus, in this study, solubility of rifaximin was improved by its complexation to ß-cyclodextrin by (i) phase solubility diagram, (ii) malaxation, and (iii) decreasing particle size by wet milling. Improved solubility provides lower doses and facilitates compliance with pharmacotherapy. The products formed were analyzed by spectrophotometry in the infrared region (FT-IR), differential scanning calorimetry (DSC), and X-ray diffraction (XRD). Also, their solubility and microbiological activity were determined. The products obtained in all techniques were more soluble than the free drug; they presented higher thermal stability and antimicrobial potency was approximately 100% with all the formulations. It is important to highlight that the treatment failure not only affects the quality of life of the patients, but also contributes significantly to the economic burden of the health system. Therefore, these findings are extremely interesting, both from a technological and financial point of view.

Evolution of green chemistry and its multidimensional impacts: A review.

The growing process of industrialization was a milestone for world economic evolution. Since the 1940s, social movements have revolutionized green chemistry and provided shifts in industrial positions and sustainable processes with advances in environmental impact and awareness of companies and population. Paul Anastas and John Warner, in the 1990s, postulated the 12 principles of Green Chemistry, which are based on the minimization or non-use of toxic solvents in chemical processes and analyzes, as well as, the non-generation of residues from these processes. One of the most active areas of Research and Development in Green Chemistry is the development of analytical methodologies, giving rise to the so-called Green Analytical Chemistry. The impacts of green chemistry on pharmaceutical analyzes, environmental, population, analyst and company are described in this review and they are multidimensional. Every choice and analytical attitude has consequences both in the final product and in everything that surrounds it. The future of green chemistry as well as our future and the environment is also contemplated in this work.