Enhancing simultaneous determination of some angiotensin II receptor antagonists and amlodipine in plasma using HPTLC with fluorescence densitometry: Independent fluorescence detection of the co-administrative drugs in the mixture across various pH conditions.

A novel and highly sensitive high-performance thin-layer chromatographic (HPTLC) method was developed and validated to quantify a combination of five pharmaceutical mixtures spiked to human plasma. The compounds comprised Amlodipine (AML) along with five angiotensin II receptor antagonist drugs (AIIRAs), namely Olmesartan (OLM), Telmisartan (TLM), Candesartan (CAN), Losartan (LOS), and Irbesartan (IRB). HPTLC was performed on silica gel 60 F254 plates using a mobile phase of Toluene: ethyl acetate: methanol: acetone: acetic acid (6:1.5:1:0.5:1, v/v/v/v/v). In a pioneering move, a reflectance/fluorescence detection mode was employed to identify two concurrently administered drugs at different pH levels for the first time. This method utilized the same chromatographic system, incorporating a specific measurement for AML at a neutral medium to achieve its maximum fluorescence at a 360 nm excitation wavelength, and measuring emission using a 540 nm optical filter. The process involved obtaining a very low fluorescence response from AIIRA. Subsequently, to enhance AIIRA's fluorescence, the plate was sprayed with perchloric acid to transition to a strong acidic medium, ultimately attaining the maximum fluorescence of AIIRA using various excitation wavelengths and a 400 nm emission filter. Through this strategic process, we could optimize the fluorescence signals of both drugs, thereby elevating the sensitivity of detection for this drug combination. AML demonstrated a linear range of 18-300 ng/band, while AIIRAs drugs exhibited a linear range of 6-150 ng/band. The method satisfied the International Conference on Harmonization (ICH) criteria for recovery, precision, repeatability, and robustness, showcasing exceptional sensitivity. The approach was successfully applied to quantify AML and AIIRAs drugs in both bulk drug and plasma samples, achieving high recovery percentages and minimal standard deviations.

Determination of antihistaminic drugs alcaftadine and olopatadine hydrochloride via ion-pairing with eosin Y as a spectrofluorimetric and spectrophotometric probe: application to dosage forms.

Four sensitive and fast analytical approaches relied on ion pairing with eosin Y were built up and evaluated using spectroscopy for determination of Alcaftadine and Olopatadine hydrochloride with high sensitivity and selectivity. Two spectrofluorimetric techniques were employed to observe the quenching effect of Alcaftadine or Olopatadine hydrochloride on the intrinsic fluorescence of eosin Y in a 0.1 M acetate buffer solution at pH 3.8 and 3.3 for Alcaftadine and Olopatadine hydrochloride, respectively. Those methods are considered the first spectrofluorimetric methods for Alcaftadine and Olopatadine hydrochloride assay. The fluorescence quenching effect was linear with concentration ranging from 150 to 2000 and 200 to 2000 ng mL-1 for Alcaftadine and Olopatadine hydrochloride, respectively. In the two spectrophotometric techniques, the absorbance of the produced ion-pair was monitored at 548 and 547 nm in aqueous buffered solution at pH 3.8 and 3.3 for Alcaftadine and Olopatadine hydrochloride, respectively. Beer's law was obeyed in the concentrations range of 0.8-8.0 and 1.0-10.0 µg mL-1. The four techniques were evaluated in accordance with ICH requirements and were effectively used to analyze dosage forms with a high percent recovery.

Development of a green synchronous spectrofluorimetric technique for simultaneous determination of Montelukast sodium and Bilastine in pharmaceutical formulations.

For the treatment of rhinitis and asthma, a combination of Montelukast sodium and Bilastine has just been approved. Based on the first derivative of synchronous fluorescence, the current work developed a green, highly accurate, sensitive, and selective spectroscopic approach for estimating Montelukast sodium and Bilastine in pharmaceutical dosage form without previous separation. The selected technique focuses on measuring the synchronized fluorescence of the studied medications at a fixed wavelength range (Δλ) = 110 nm, and using the amplitude of the first derivative's peak at 381 and 324 nm, for quantitative estimation of Montelukast sodium and Bilastine, respectively. The impacts of different factors on the referred drugs' synchronized fluorescence intensity were investigated and adjusted. The calibration plots for were found to be linear over concentration ranges of 50-2000 ng mL-1 for Montelukast sodium and 50-1000 ng mL-1 for Bilastine. Montelukast sodium and Bilastine have LODs of 16.5 and 10.9 ng mL-1, respectively. In addition, LOQs were: 49.9 and 33.0 ng mL-1, for both drugs, respectively. The developed method was successfully employed to quantify the two drugs in synthetic tablets mixture and in laboratory prepared mixtures containing varied Montelukast and Bilastine ratios. To compare the results with the published analytical approach, a variance ratio F-test and a student t-test were used, which revealed no significant differences.

Ultrasensitive TLC determination of montlukast and loratadine mixture in human plasma utilizing fluorescence detection at dual pH values: Toward attaining separate maximum fluorescence intensity.

A novel selective and highly sensitive TLC densitometric method with reflectance/fluorescence detection was developed to separate and quantify montlukast (MONT) and loratadine (LOR). Separation of the studied drugs was performed on precoated silica gel TLC plates using chloroform-ethyl acetate (8 :2 v/v) as a mobile phase. MONT quantification was carried out by measuring emission using 400 nm optical filter after excitation at 340 nm. Enhancement of the week LOR fluorescence was performed through adequate spraying the chromatograms with 0.2 M perchloric acid leading to enhancing sensitivity by 17 folds compared to the reported HPTLC methods with absorbance detection. The scanner was set at 275 nm excitation wavelength and 400 nm optical filter. Detection of both drugs on the same plate separately at different pH conditions was utilized for the first time. Maximum fluorescence was achieved for each of them and this enhances detection sensitivity for both drugs. The linear regression analysis data of the studied drugs produced a good linear relationship with correlation coefficients of 0.996 for MONT and 0.998 for LOR over the concentration range of 6 - 150 ng/band for MONT and 15 - 120 ng/band for LOR. Limit of detection values were 1.7 and 4.5 ng /band for MONT and LOR respectively. The developed method enabled the detection of MONT and LOR in human plasma samples within linear concentrations ranged from 7 to 140 ng/ band and 16 to 50 ng/ band with detection limits of 1.9 and 4.8 ng/band for MONT and LOR respectively. The analytical performance of the proposed method was evaluated according to the International Council for Harmonization (ICH). The method was successfully applied for the analysis of the studied drugs in spiked human plasma and good recovery percentages were obtained indicating that there is no interference from plasma constituents. Therefore the method can be applied for in vivo analysis and pharmacokinetic study.

HPTLC Method for the Ultrasensitive Detection of Triamterene in Plasma.

A high-performance thin-layer chromatographic (HPTLC) method has developed for the selective detection of a diuretic drug, triamterene (TRIAM), in pure form, tablets and human plasma. The method was based on chromatographic separation of TRIAM using HPTLC plates, precoated with silica gel, and a mobile phase consisted of ethyl acetate: dimethylformamide: ammonia (7.0: 2.7: 0.3, by volume). The native fluorescence signal of TRIAM was detected at 440 nm and used to quantify TRIAM using the proposed method, improving the method sensitivity to ~250-folds in comparison to that reported in previous HPTLC studies. The developed method enabled the detection of TRIAM in pure drug and biological samples (human plasma) within linear concentrations ranged from 0.8 to 60 ng/band or 1.0 to 60 ng/band for pure drug and plasma samples, respectively. Furthermore, the method was validated according to the official guidelines to permit its applicability in quality control and clinical laboratories.

An epidermal patch for the simultaneous monitoring of haemodynamic and metabolic biomarkers.

Monitoring the effects of daily activities on the physiological responses of the body calls for wearable devices that can simultaneously track metabolic and haemodynamic parameters. Here we describe a non-invasive skin-worn device for the simultaneous monitoring of blood pressure and heart rate via ultrasonic transducers and of multiple biomarkers via electrochemical sensors. We optimized the integrated device so that it provides mechanical resiliency and flexibility while conforming to curved skin surfaces, and to ensure reliable sensing of glucose in interstitial fluid and of lactate, caffeine and alcohol in sweat, without crosstalk between the individual sensors. In human volunteers, the device captured physiological effects of food intake and exercise, in particular the production of glucose after food digestion, the consumption of glucose via glycolysis, and increases in blood pressure and heart rate compensating for oxygen depletion and lactate generation. Continuous and simultaneous acoustic and electrochemical sensing via integrated wearable devices should enrich the understanding of the body's response to daily activities, and could facilitate the early prediction of abnormal physiological changes.

Epidermal Enzymatic Biosensors for Sweat Vitamin C: Toward Personalized Nutrition.

Recent advances in wearable sensor technologies offer new opportunities for improving dietary adherence. However, despite their tremendous promise, the potential of wearable chemical sensors for guiding personalized nutrition solutions has not been reported. Herein, we present an epidermal biosensor aimed at following the dynamics of sweat vitamin C after the intake of vitamin C pills and fruit juices. Such skin-worn noninvasive electrochemical detection of sweat vitamin C has been realized by immobilizing the enzyme ascorbate oxidase (AAOx) on flexible printable tattoo electrodes and monitoring changes in the vitamin C level through changes in the reduction current of the oxygen cosubstrate. The flexible vitamin C tattoo patch was fabricated on a polyurethane substrate and combined with a localized iontophoretic sweat stimulation system along with amperometric cathodic detection of the oxygen depletion during the enzymatic reaction. The enzyme biosensor offers a highly selective response compared to the common direct (nonenzymatic) voltammetric measurements, with no effect on electroactive interfering species such as uric acid or acetaminophen. Temporal vitamin C profiles in sweat are demonstrated using different subjects taking varying amounts of commercial vitamin C pills or vitamin C-rich beverages. The dynamic rise and fall of such vitamin C sweat levels is thus demonstrated with no interference from other sweat constituents. Differences in such dynamics among the individual subjects indicate the potential of the epidermal biosensor for personalized nutrition solutions. The flexible tattoo patch displayed mechanical resiliency to multiple stretching and bending deformations. In addition, the AAOx biosensor is shown to be useful as a disposable strip for the rapid in vitro detection of vitamin C in untreated raw saliva and tears following pill or juice intake. These results demonstrate the potential of wearable chemical sensors for noninvasive nutrition status assessments and tracking of nutrient uptake toward detecting and correcting nutritional deficiencies, assessing adherence to vitamin intake, and supporting dietary behavior change.

Electrochemical determination of antihypertensive drugs by employing costless and portable unmodified screen-printed electrodes.

Hypertension increases the risk of heart disease and stroke, is commonly known as a silent killer disease and considered as one of the key risk factor for premature death and disability over the world. Herein, we report for the first time a sensitive, costless and reproducible voltammetric method for individual determination of five antihypertensive drugs namely, propranolol (PRO), timolol (TIM), amlodipine (AML), amiloride (AMI) and triamterene (TRI) using differential pulse voltammetry at bare/unmodified screen-printed carbon electrodes (SPEs) in presence of sodium dodecyl sulfate (SDS). Each drug exhibits an electrochemical signal in aqueous media which is significantly enhanced in presence of optimized concentration of SDS due to accumulation of the protonated drug molecules and electrostatically interaction with negatively charged micellar structures. As a result, the spherical micellar orientation of SDS onto the graphitic surface of SPEs offered the analytically sensitive determination of the target drugs over a wide linear concentration range with nano-molar detection limits possible negating the need for any complicated surface modifications. Finally, the proposed voltammetric method was successfully utilized in the individual determination of the target antihypertensive drugs in pharmaceutical formulations and human urine samples.

Two selective HPTLC methods for determination of some angiotensin II receptor antagonists in tablets and biological fluids.

Two simple, selective, precise and highly sensitive high-performance thin-layer chromatography (HPTLC) methods have been developed and validated for analysis of five angiotensin II receptor antagonists, namely losartan, irbesartan valsartan, candesartan and olmesartan, which are widely used in clinical practice. HPTLC of the drugs was performed on pre-coated silica gel HPTLC plates 60 F254 by development using a mobile phase composed of chloroform-acetone-glacial acetic acid (7.8:1.5:0.7m v/v/v), which was suitable for all of the studied drugs. The first method depended on utilizing reflectance/fluorescence mode for detection while the second method depended on using 2,3,5,6-tetrachloro-1,4-benzoquinone as spraying reagent for the first time to form orange spots scanned at 460 nm. A good linear relationship was obtained over the concentration ranges of 1.2-60 and 360-3000 ng/band while detection and quantification limits were in the ranges of 0.07-0.43, 45.2-140.49 and 0.21-1.29, 137.05-425.74 ng/band for reflectance/fluorescence and reflectance/absorbance methods respectively. The developed methods were applied successfully for their determination in tablets and spiked human plasma for reflectance/fluorescence method with good accuracy and precision, and so can be applied in the pharmacokinetic and bioavailability studies.