Trichloroacetic Acid Solution Research Articles

Simultaneous determination of colistin sulfate and tigecycline in human plasma by liquid chromatography-tandem mass spectrometry method

ObjectiveTo establish a high-performance liquid chromatography–tandem mass spectrometry method (HPLC–MS/MS) to simultaneously determine colistin sulfate and tigecycline in human plasma.MethodsPolymyxin B1 internal standard (20 µL) was added into 200 µL of plasma sample. The samples were treated with methanol-5% trichloroacetic acid (50:50, V/V) solution, and the protein precipitation method was adopted for post-injection analysis. The chromatographic column was a Dikma C18 (4.6 mm × 150 mm, 5 μm). For the mobile phase, 0.1% formic acid in aqueous solution was used for phase A, 0.1% formic acid in acetonitrile solution for phase B, and gradient elution was also applied. The flow rate was 0.8 mL/min, the column temperature was 40 °C, and the injection volume was 10 µL; Electrospray ionization and multiple reaction ion monitoring were adopted and scanned by the HPLC–MS/MS positive ion mode.ResultsThe endogenous impurities in the plasma had no interference in the determination of the analytes. There existed a good linear relationship of colistin sulfate within the range of 0.1–10 µg/mL (R2 = 0.9986), with the lower limit of quantification (LLOQ) of 0.1 µg/mL. There existed a good linear relationship of tigecycline within the range of 0.05–5 µg/ mL (R2 = 0.9987), with the LLOQ of 0.05 µg/mL. The intra- and inter-day relative standard deviations of colistin sulfate and tigecycline were both less than 15%, and the accuracy was between 88.21% and 108.24%. The extraction had good stability, the extraction recovery rate was 87.75–91.22%, and the matrix effect was 99.40–105.26%.ConclusionThis study successfully established a method for simultaneously detecting colistin sulfate and tigecycline plasma concentrations. The method was simple, rapid, and highly sensitive and could be applied for therapeutic medication monitoring.

Evidence-based management of cutaneous scarring in dermatology part 2: atrophic acne scarring.

Atrophic acne scars are the most common type of acne scars and are classified into three main types: icepick, boxcar, and rolling scars. Various procedures and techniques for atrophic acne scarring are discussed in detail, with stronger evidence-based support for lasers (non-fractional, fractional, ablative, and non-ablative), platelet-rich plasma as adjunctive treatment, chemical peels (glycolic acid, trichloroacetic acid, and Jessner's solution), dermal fillers such as hyaluronic acid, and microneedling, and lesser quality evidence for microdermabrasion, subcision, and lipoaspirate grafting. Further research is needed to optimize treatment protocols, assess the efficacy of monotherapies, and establish standardized guidelines for clinicians. This paper will provide a comprehensive review of the evidence-based management of atrophic acne scars, including currently commonly utilized therapies as well as more innovative treatment options.

Towards Formulation of Highly Acidic Active Ingredients: Development of Clinically Effective Concentrated Trichloroacetic Acid Gel for Wart Management.

Common warts are benign skin lesions caused by the human papillomavirus. Although they are usually not harmful, they can cause pain, depending on their location. While many modalities are available for treatment of warts, none is a gold standard, and many are not affordable and/or have suboptimal outcomes. Trichloroacetic acid (TCA) is a chemical tissue-destroying agent used as a highly concentrated solution for wart management. While available and efficient, it is difficult to handle as the solution spreads to tissue surrounding the wart causing pain and burning. Hence, we developed a new polymer-based gel of high TCA content (100% w/v). Gels were formed successfully as hydroxyethyl cellulose (HEC) and chitosan were used to impart viscosity and bioadhesion. Formulae of different concentrations were tested for their physical properties, and the optimal formulation was selected for clinical evaluation. A combination of 3% HEC and 2% chitosan provided optimal viscosity and limited water content and have acceptable stability. The efficacy and safety of the biweekly application of TCA gel were evaluated in 30 patients. The clinical study revealed gel's efficacy and tolerability; half of the patients showed a complete cure, and 90% showed improvement within 6weeks. Only 10-12% of the patients reported side effects. In summary, transforming TCA solution into a gel enabled its application and handling in a practical manner by physicians and patients alike, while maintaining its efficacy as a tissue-destroying agent. Moreover, it is economic and easy to apply, rendering it a promising formulation for similar conditions requiring controlled tissue ablation.

Microextraction of Tigecycline Using Deep Eutectic Solvents and Its Determination in Milk by LC-MS/MS Method.

The occurrence of tigecycline (TGC), a new first glycylcycline antibiotic residues in food products harmfully influences potential human consumers health. Therefore, analysts are forced to develop new microextraction methods connected with modern extractants for effective isolation of this compound. For this purpose, deep eutectic solvents (DES) as the extraction media were used. Liquid-liquid microextraction (LLME) of tigecycline from milk samples with application of the hydrophobic deep eutectic solvents: decanoic acid:thymol (1:1), thymol:camphor (2:1), dodecanoic acid:menthol (2:1), and dodecanoic acid:dodecanol (1:1) was developed. The studied samples were subjected to a deproteinization process using trichloroacetic acid solution and acetonitrile. The optimal microextraction parameters, molar ratio of DES components, amount of extraction solvents, pH of milk sample, shaking, and centrifugation time, were chosen. Tigecycline in the obtained microextracts of deep eutectic solvents was analyzed using a liquid chromatographic technique connected with a tandem mass spectrometry (LC-MS/MS) system. The limits of detection and quantification values for TGC determination followed by DES-LLME-LC-MS/MS method were in the 1.8 × 10-11 mol L-1 (0.01 μg kg-1) to 4.0 × 10-9 mol L-1 (2.28 μg kg-1) and 5.5 × 10-11 mol L-1 (0.03 μg kg-1) to 1.2 × 10-8 mol L-1 (6.84 μg kg-1) ranges, respectively. The RSD values of precision were in the range 1.4-7.8% (intraday) and 5.4-11.7% (interday). The developed procedures were used for the determination of tigecycline in different bovine milk samples.

DEVELOPMENT OF METHOD FOR QUANTITATIVE DETERMINATION OF CEFQUINOME SULFATE IN PIGLETS BLOOD PLASMA USING HPLC/DMD

This manuscript presents a developed method for determining cefquinome sulfate in piglets blood plasma intended for clinical and pharmaceutical research of veterinary drugs based on it. Blood plasma proteins were precipitated twice with a solution of trichloroacetic acid. The supernatant was further purified by a series of solid-phase extraction. Separation was performed on an inverted phase Kinetex EVO С18 column using acetonitrile and 0,1 % trifluoroacetic acide solusion as the mobile phase. The gradient mode of eluents was used during 10 min at a flow rate of 1,4 ml/min. The peak retention time of cefquinome sulfate is 4,2 min. The specificity of the analytical method was checked by comparing the chromatographic separation of a sample of blood plasma enriched with a standard solution of cefquinome sulfate and a sample of blood plasma placebo. The preparing loaded blood plasma samples procedure for building a calibration graph is described in the article. The validation parameters of the method “recovery” and “coefficient of variation” were considered in accordance with the criteria of Council Directive 2002/657/EC. The procedure of sample preparation of fortified blood plasma to construct calibration graph is described in the manuscript. The mean recovery from fortified blood plasma samples in the range of 0.1-2.0 μg/ml cefquinom sulfate was 102.3 %. The method is linear in the concentration range of 0.1 – 4.0 μg/ml of cefquinome sulfate. The correlation coefficient for the determination method is 0.9998. The results obtained in the study of the linearity of this technique were used to estimate the correctness and convergence. The accuracy of the measurements was evaluated by examining the known amounts of analyte added to the control blood plasma. Recovery data are acceptable because they are within ± 10% of the target value. The method has sufficient convergence (accuracy). The evaluation of the intermediate precision of cefquinome sulfate determination was assessed on three different days of analysis. The limit of detection for cefquinom sulfate is 0.05 μg/ml and limit of quantification - 0.10 μg/ml. The average CV for each compound was <10%. The procedure was confirmed and then applied to determination cefquinome sulfate in the pig blood plasma obtained during the study of the pharmacokinetics of the veterinary drug. The HPLC/DMD method can be used for study of the pharmacokinetics of the veterinary drug.

Development of conditions for sertraline isolation from biological fluids

The toxicological significance of antidepressant drugs is steadily increasing. Development of the effective methods of the sample preparation is a topical issue of the chemical-toxicological analysis of antidepressants. Aim. To develop conditions for isolating the antidepressant sertraline from the blood and urine by the liquid-liquid extraction. Materials and methods. The studies were performed with model blood and urine samples spiked with sertraline. In the study of the blood, the formed blood elements were pre-precipitated by adding a 10 % solution of trichloroacetic acid. Extraction purification was performed with hexane at pH 1, and the drug was extracted from biological fluids with chloroform at pH 8. The extracts obtained were further subjected to the TLC purification. Determination of sertraline in eluates from chromatograms was performed by the UV spectrophotometric method. Results and discussion. The Rf value of sertraline in the mobile phase of methanol – 25 % ammonium hydroxide solution (100:10.5) was 0.42 ± 0.02. The UV spectra of the eluates from the chromatograms had absorption maxima at wavelengths of 268 ± 2, 275 ± 2 and 283 ± 2 nm and matched with the UV spectrum of a standard solution of sertraline in 0.1 mole/L ethanol solution of hydrochloric acid. The quantitative determination was performed at λmax 275 nm according to the equation of the calibration curve y = 0,00216x–0,03. The methods developed allowed to isolate 80.0 ± 4.0 % of sertraline from the urine, 39.0 ± 2.0 % from the blood serum, and additionally 8.0 ± 0.7 % of the antidepressant studiedfrom the blood sediment after its separation from the blood serum. Conclusions. The effective conditions for the sample preparation of biological fluids using the liquid-liquid extraction method for the antidepressant sertraline have been determined. The results obtained are of practical importance for creating an algorithm for the toxicological study of biological samples for the presence of this antidepressant in case of fatal drug intoxications.

Eupatorium Adenophora (Spreng.) leaves Extract as a Highly Efficient Eco-friendly Inhibitor for Steel Corrosion in trichloroacetic acid Solution

Eupatorium Adenophora (Spreng.) leaves Extract as a Highly Efficient Eco-friendly Inhibitor for Steel Corrosion in trichloroacetic acid Solution

Ion-pair hollow fiber liquid-phase microextraction combined with capillary electrophoresis for the determination of biogenic amines in rat tissues

Herein, the development of an ion-pair hollow fiber liquid-phase microextraction (IP-HF-LPME) procedure followed by capillary electrophoresis (CE) with indirect UV detection for the simultaneous extraction and determination of aliphatic biogenic amines including spermidine, spermine, and cadaverine in tissue samples of rat is described. In this study, tissue samples were firstly homogenized with a cold trichloroacetic acid solution then the developed method was applied to the supernatant resulting from tissue homogenization. Different CE separation and indirect UV detection conditions, as well as IP-HF-LPME extraction conditions were studied in detail and optimized. A 11 mmol L−1 imidazole solution containing 13 % (v/v) ethanol adjusted at pH 3.3 (by acetic acid) was the best running buffer for indirect UV detection of non-UV-absorbing amines. 1-Octanol in combination with salicylic acid, respectively as the membrane solvent and ion-pair reagent provided the highest extraction recovery for the studied amines. Method performances were established and good results of linearity, recovery, sensitivity, and repeatability were achieved for all the studied amines. Limits of detection were found to be between 2.8 and 4.5 ng mL−1 and limits of quantification were 15 ng mL−1 and the dynamic range was 15–2000 ng mL−1 for all three analytes.

Pilot Study on the Effect of a Single Topical Application of Trichloroacetic Acid 85% on Normal Cervical Tissue.

Background: Early detection and treatment of cervical intraepithelial neoplasia (CIN) through a “see and treat” approach is a pillar of cervical cancer prevention programs in developing countries such as Indonesia. One of the major challenges faced is the limited N2O or CO2 gas supply for cryotherapy. Thus, an alternative therapeutic method such as trichloroacetic acid (TCA) topical application is needed as an alternative solution. The effectiveness of this therapy will depend on its destructive effect on eliminating the whole lesion in CIN. Objective: To estimate the extent of damage in the normal cervical tissue after a single topical application of 85% TCA solution. Design and Methods: This research was an intervention study carried out by applying ±5 ml of 85% TCA solution into the cervix of 40 patients scheduled for total hysterectomy for indications other than cervical pathology 24 h before surgery. The extent of tissue destruction was determined microscopically using histopathological specimens. The study protocol is registered at www.clinicaltrial.gov (ID NCT04911075). Results: In the final analysis, 39 subjects were included. The necrotic area was detected at the superficial layer, accompanied by the full epithelial erosion thickness. In addition, there were also fibrotic areas resembling burned tissue in the stroma. The mean depth of destruction was 1.16 ± 0.01 mm in the anterior lip and 1.01 ± 0.06 mm in the posterior lip. There was no significant depth difference between the anterior and posterior lips (p ≥0.05). Moreover, the 85% TCA topical application was tolerable, as represented by the fact that the vast majority (82.1%) of participants experienced pain with a visual analog scale score of <4. Conclusion: Single dose of TCA 85% in topical solution was able to destroy the normal cervical tissue with a deeper mean depth than the mean depth of CIN III in squamous epithelium.

Carrier-Free Deferoxamine Nanoparticles against Iron Overload in Brain

Carrier-Free Deferoxamine Nanoparticles against Iron Overload in Brain

Dissolution kinetics of malachite in trichloroacetic acid solution

Dissolution kinetics of malachite in trichloroacetic acid solution

Painting CROSS TCA technique: Modification of the CROSS method for the treatment of atrophic acne scars-Case series.

The Chemical Reconstruction of Skin Scars (CROSS) technique was first described in 2002 and has since demonstrated safety and efficacy in multiple studies. We describe the treatment of six patients with a modified version of the CROSS method-the Painting CROSS trichloroacetic acid (TCA) technique. This technique has the advantage of offering even higher tissue selectivity and better control of the scar edges, enhancing both safety and efficacy. We retrospectively evaluated 31scars of six patients who underwent a single treatment by the Painting CROSS TCA method. A 0.3ml insulin syringe with a 30-gauge needle was filled with 0.05ml of 85% TCA solution and then applied to the scar base with slight pressure until frosting was achieved. Patients were evaluated before and 3months after treatment for scar volume deficit by a high-resolution three-dimensional imaging system. The average volume of the 31scars assessed in our study was 2.71mm3 before treatment and 1.96mm3 after treatment. There was a 26.3% average decrease in the volume of the scars after one treatment. Transient mild hyperpigmentation was noted in two patients after the treatment. Painting CROSS TCA technique has demonstrated efficacy in the treatment of acne scars after a single treatment.

Comparative study of technologies for extraction of biologically active substances from the raw material of animal origin

Technologies of isolation and concentration of biologically active substances, developed in the middle of the 20th century, need adjustment and adaptation to modern conditions both to increase the activity of substances and for greater economic efficiency. The aim of the research is the comparison of dynamics of biologically active compounds extraction from porcines pancreas in two methods: the saline method based on 0.9% sodium chloride solution, and the acidic method based on 2.4% trichloroacetic acid solution. Also the purpose of research is to assess the possibilities for further optimization of technologies. The total protein concentration based on the biuret reaction in the samples taken during the extraction, as well as the calculation and analysis of the point degrees and rates of extraction are chosen as the controlled parameters. Local maxima of the protein yields into the extractant media at the 60th, 135th and 255th minute were recorded during saline extraction; and at the 75th and 135th minute during acid extraction. Also the proteomic profile of the extracts was studied. Wide range of compounds with molecular weight of less than 52 kDa was found in extracts based on physiological saline solution, and protein substances of whole presented range of molecular weights in trichloroacetic acid based extracts were considered. The predominance of low molecular weight protein fraction of interest was noted also in this method of extraction in comparison with the other methods of extraction. According to the UniProt database, we assume availability of probable compounds with a molecular weight of less than 30 kDa in the purified acidic extract. The presence of some proteins absent in the final saline extract was noted. The acidic erythrograms showed a weak degrading effect of both types of extracts on the membranes of rat erythrocytes, as well as the cytoprotective effect of acidic ultrafiltrates (less than 3 kDa). The obtained results prove a better efficiency of trichloroacetic acid extraction method used for obtaining a mixture of a wide range of compounds, including biologically active substances of low molecular weight.

Physicochemical Properties Of 131I-Rutin Under Acidic Labeling Condition As A Radiolabeled Compound For The Diagnosis Of Cancer

Radiolabeled rutin (131I-rutin) has potential use in future diagnosis of cancer. The physicochemical characteristics of 131I-rutin are essential in regard to its distribution and accumulation in the body. Therefore, to ensure successful delivery of a labeled compound, it is necessary to evaluate its physicochemical properties. The labeling of 131I-rutin was accomplished using the oxidation method assisted by Chloramine-T under acidic conditions. Radiochemical purity value was measured by thin-layer chromatography (TLC-SG F254) using 100% methanol as the mobile phase. The electrical charge of 131I-rutin was determined by the paper electrophoresis. Moreover, the lipophilicity (P) was evaluated by the partition coefficient in the organic-water liquid. Plasma protein binding was determined in vitro by precipitation method using a 5% trichloroacetic acid (TCA) solution. The results showed that 131I-rutin has a neutral charge and a lipophilicity value (Log P) of 0.395 ± 0.203 (hydrophilic), and was bound to human blood plasma proteins with a percentage of 69.36% ± 1.88%.

Leaching Kinetics of Lead from Galena Using Hydrogen Peroxide and Trichloroacetic Acid

Abstract The leaching kinetics of lead (Pb) from galena using hydrogen peroxide (H2O2) in trichloroacetic acid (TCA) solution will be explored in this study. The influence of temperature, stirring ...

Laboratory toxicological diagnosis of trazodone intoxications

When determining the cause of poisoning by antidepressant drugs, the data of laboratory toxicological studies of biofluids for the presence of this group of drugs are of key importance. Aim. To develop the methods for determining the antidepressant drug trazodone in the blood and urine samples using high-performance liquid chromatography with a UV spectrophotometric detection, which is suitable for analytical diagnosis of the thymoleptics intoxications. Materials and methods. The model samples of human biofluids spiked with trazodone were studied. The antidepressant was isolated from the blood and urine by the liquid-liquid extraction with methylene chloride from the alkaline medium at pH 9. Concomitant endogenous impurities were removed by extraction with diethyl ether from the acidic medium at pH 1. In the study of the blood the erythrocyte mass was pre-precipitated with the help of 10 % of trichloroacetic acid solution. Chromatographic analysis was performed on a microcolumn chromatograph using a column with a reversed-phase of C18. Results. The absolute retention time of trazodone in extracts from the model samples of biofluids was 17.91±0.09 min. The quantitative content of trazodone was determined at 250 nm by the calibration dependence of the chromatographic peak area on the concentration (μg/ml) y=(1.74∙10-3±1∙10-5)x. Under the indicated extraction conditions, 35±4 % and 78±4 % of trazodone were isolated from the blood and urine, respectively. Conclusions. The methods of trazodone isolation from the biofliuds by liquid extraction followed by the determination of the drug by high performance liquid chromatography with a multiwave UV spectrophotometric detection have been developed. The methods are recommended for using in the practice of forensic and clinical toxicology.

Adsorption and Inhibition Behavior of Imidazoline on Steel Surface in Trichloroacetic Acid Solution

Adsorption and Inhibition Behavior of Imidazoline on Steel Surface in Trichloroacetic Acid Solution

The development of the conditions for vortioxetine isolation from biological fluids

The chemical-toxicological significance of antidepressant drugs is steadily increasing. The development of effective methods of the sample preparation of the biological material is an important analytical aspect in toxicology of the newgeneration antidepressants. Aim. To develop the conditions for the sample preparation of biological fluids in order use them in the chemicaltoxicological analysis of the new antidepressant vortioxetine. Materials and methods. The studies were performed with model blood and urine samples spiked with vortioxetine. When examining the blood the formed blood elements were pre-precipitated by adding 10 % solution of trichloroacetic acid. The extraction purification was performed with hexane at pH 1-2, and the drug was extracted from the biologicalfluids with methylene chloride at pH 8-9. The extracts obtained were further subjected to TLC purification. Vortioxetine in eluates from chromatograms was determined by the UV-spectrophotometric method. Results and discussion. The Rf value of vortioxetine in the mobile phase of ethyl acetate-methanol-25 % ammonium hydroxide solution (85 : 10 : 5) was 0.77 ± 0.05. The UV spectra of the eluates from the chromatograms had absorption maxima at the wavelengths of 229 ± 2 and 232 ± 2 nm and matched with the UV spectrum of the standard solution of vortioxetine in methanol. The quantitative determination was performed at λmax232 nm by the equation of the calibration curve y = (0.0172 ± 3 · 10-4)x + (0.027 ± 0.008). Under the conditions of the sample preparation developed 27 ± 1 % of vortioxetine from the blood and 62 ± 2 % of the drug from the urine were isolated. Conclusions. The efficiency of the sample preparation of biological fluids by the method of liquid-liquid extraction in relation to the new antidepressant vortioxetine has been determined. The methods developed are recommended for use in forensic and clinical toxicology.

Synergistic inhibition effect of walnut green husk extract and potassium iodide on the corrosion of cold rolled steel in trichloroacetic acid solution

Plant extract inhibitor is of low price, rich natural raw resources, eco-friendly and biodegradable. To further strengthen inhibition stability and efficiency, halide ion is always mixed with plant extract so as to produce synergism. In the present work, the synergistic inhibition effect of walnut green husk extract (WGHE) and potassium iodide (KI) on the corrosion of cold rolled steel (CRS) in trichloroacetic acid (Cl3CCOOH) solution was studied by weight loss, electrochemical techniques and surface analysis. Results show that WGHE moderately inhibits the corrosion of CRS in Cl3CCOOH media. However, WGHE/KI mixture has pleasant inhibitive ability with the maximum inhibition efficiency of 97.2% in 0.10 M Cl3CCOOH from weight loss method. There is a synergism for WGHE mixing with KI, and all corresponding synergism parameters are high than unity. The adsorption of WGHE either in the absence or presence of KI obeys Langmuir adsorption isotherm, and the external addition of KI facilitates the adsorption of WGHE on steel surface. Individual WGHE mainly retards cathodic reaction, while WGHE/KI mixture drastically inhibits both anodic and cathodic reactions simultaneously. Nyquist appears a capacitive loop at high frequencies followed by an inductive loop at low frequencies. The charge transfer resistance follows the order: WGHE/KI > KI > WGHE. SEM and AFM clearly proves the corrosion degree and surface roughness of CRS surface were dropped to more extent with the synergistic WGHE/KI mixture. Moreover, the synergistic inhibition of two main components of juglone and kaempferol with KI was discussed in detail under same conditions.

Evaluation of tetracycline, oxytetracycline and penicillin G residues in chicken meat samples by high performance liquid chromatography with pda detection

Penicillin G, tetracycline and oxytetracycline are broad-spectrum antibiotics with considerably low side effects which are used in most of the poultries. Due to complex matrix effects, it is considerably difficult to isolate these compounds from other molecules (such as proteins and lipids) in order to analyze. In this study, a high performance liquid chromatography (HPLC) coupled with photodiode array (PDA) detector system was introduced for the determination of tetracycline, oxytetracycline and penicillin G residues in nine chicken breast samples. For the separation of tetracycline and oxytetracycline out of samples prior to the analysis, trichloroacetic acid (TCA) and McIlvaine buffer solutions were used while formic acid and phosphate buffer solutions were utilized for penicillin G using a solid phase extraction system. The peaks at the chromatograms were enlightened and recovery percentages were calculated using spiked samples (96.57% for penicillin G; 99.00% for oxytetracycline; 95.92% for tetracycline). LOD and LOQ values were calculated, respectively as 1.55 gL-1 and 5.20 gL-1 for tetracycline; 1.32 gL-1 and 4.39 gL-1 for oxytetracycline; 1.07 gL-1 and 3.60 gL-1 for penicillin G. With the proposed method, the determination of three antibiotic residues was performed in less than 15 minutes and applied successfully to real samples.