Drugs In Human Urine Research Articles

Facile fabrication of the immuno-MALDI-MS chip for the enrichment of abused drug in human urine integrated with MALDI-MS analysis

BackgroundDrug abuse can result in both physical and mental health issues for individuals, and can also contribute to broader societal problems. The number of drug abuse cases rose to 296 million in 2021. The sample pretreatment methods commonly employed typically require longer processing times and occasionally necessitate derivatization. Furthermore, with the increase in sample sizes, traditional chromatography-mass spectrometry methods for analyzing abused drugs were no longer sufficient to handle such numerous samples. In this study, immuno-MALDI-MS chip were fabricated for specific enrichment of illicit drugs, integrating with the rapid and accurate capabilities of MALDI-MS for high-throughput analysis of drug abuse. ResultsThe immuno-MALDI-MS chip was successfully prepared by coating an aluminum chip with antibody-conjugated boronic acid-modified gold nanoparticles. Ketamine, a frequently abused illicit drug, served as the proof of concept for this study. The immuno-MALDI-MS chip was employed to selectively enrich ketamine in human urine samples, facilitating direct MALDI-MS analysis with the addition of α-CHCA matrix solution. The challenge of detecting abused drugs, exacerbated by interfering peaks in the low m/z region from salts and small molecules in human urine samples, was successfully overcome. The developed method exhibited a wide linear range of 10–5000 ng/mL with a limit of detection of 3.3 ng/mL for ketamine. Notably, the proposed method enabled high-throughput screening and accurate confirmation of ketamine concentrations in suspects' urine samples within few minutes, requiring a minimal sample volume of 1 μL. The obtained data were in complete agreement with the previous GC/MS analysis. SignificanceA straightforward, cost-effective and sensitive method for the selective enrichment and absolute quantification of abused drugs was developed using a homemade immuno-MALDI-MS chip integrated with MALDI-MS analysis. This method combines the advantages of immunoassay and mass spectrometry, offering both speed and accuracy. The reported method for the quantification of ketamine in human urine offers a practical approach and has the potential to analyze emerging new psychoactive substances in the future.

Elucidating important factors and corresponding method optimization for sensitive detection of small peptide drugs in human urine by solid-phase extraction and UPLC-HRMS: The influence of MS scan modes, protein precipitants, and ammonium formate.

Small peptide hormones are widely used in sports as performance-enhancing substances, making it crucial to develop sensitive analytical methods for their detection in doping control analysis. Various factors significantly affect analytical sensitivity, such as the selection of ultra-performance liquid chromatography (UPLC) mobile phase, high-resolution mass spectrometry (HRMS) scanning modes, and extraction solvents for pretreatment. Herein, comparative study approach was utilized to investigate the sensitivity of each peptide analyte under both full scan and parallel reaction monitoring (PRM) modes of HRMS and assess the effects of some protein precipitants as a part of extraction solvents on solid-phase extraction (SPE). The results showed that full scan should be selected as the primary scan mode of HRMS, and the combination with PRM mode could effectively compensate for the limitations of full scan, and the addition of protein precipitants would adversely affect the detection of certain small peptide analytes. Meanwhile, influences of ammonium formate in reverse UPLC mobile phase on the charge state distribution of small peptides were investigated and elucidated. Based on these findings, a sensitive and reliable UPLC-HRMS analytical method combining full scan and PRM mode was validated for screening and confirmation of 63 small peptide analytes after SPE, with limits of detection (LODs) ranging between 0.010 and 0.473 ng/ml and limits of identification (LOIs) ranging between 0.015 and 1.512 ng/ml. Additionally, suggestions were provided for the detection of [Arg8]-vasopressin, dermorphin, and its analogues.

Reversible switchable deep eutectic solvent for dispersive liquid–liquid microextraction of non-steroidal anti-inflammatory drugs in biological and wastewater samples combined with high-performance liquid chromatography

The development of fast and simple bioanalytical methods for determining drugs is increasing. In the present study, a pH-induced reversible switchable deep eutectic solvent based on dispersive liquid–liquid microextraction was assessed (sDES-DLLME) for the analysis of three non-steroidal anti-inflammatory drugs (salicylic acid, mefenamic acid, and diclofenac) in plasma, urine and wastewater samples and their analysis by high-performance liquid chromatography. In this study, the switching process of DES (sDES) composed of 2-isopropyl-5-methylphenol (thymol) and a fatty acid was performed by pH adjustment. By adding NaOH to the sample solution, a homogeneous phase was achieved based on the hydrophilic form of sDES, and a two-phase system was obtained by adding an inorganic acid (HCl) to return the hydrophobicity. The important factors, such as DES type, the DES volume and the conditions of NaOH and HCl solutions were perused. Under optimal conditions, the limits of detection and limits of quantification were acquired in the range from 1 to 3 μg L−1 and 3 to 9.2 μg L−1 for three analytes, respectively. The ER% and EF values were to be in the range of 93.3 to 97.2 % and 112 to 117 for all analytes. A good linear range was declared up to 500 μg L−1 while the precision (%RSD) as the inter-day and intra-day in different samples was in the range of 4.6–6.1 % and 2.7–5.1 % respectively. Subsequently, the developed method was utilized to analyze the drugs in human urine, plasma and wastewater samples.

Salicylic acid as a switchable hydrophilicity solvent for the microextraction of the antibiotic amphotericin B from human urine followed by HPLC-UV analysis

Monitoring the concentration levels of amphotericin B in the human organism is of utmost importance to evaluate the efficacy of the therapy. However, the reported sample preparation protocols for the extraction of this compound are very limited. In this work, salicylic acid is utilized as a switchable hydrophilicity solvent for the microextraction of amphotericin B from human urine samples before the HPLC analysis. The method is based on the phase transition of salicylic acid by changing the pH of the sample enabling efficient dispersion and phase separation in one step. A high contact area of the solidified solvent with the sample solution provided effective extraction of the target analyte. Among others, critical experimental parameters affecting the extraction performance of the drug were systematically investigated. The separation of the drug was carried out on a C8 stationary phase using mixtures of citric acid and methanol as mobile phases. Excellent linearity was observed in the range of 0.1 – 2.0 μg mL−1, while the precision (%RSD) was less than 14.5 % in all cases. The lower limit of quantification was 0.1 μg mL−1, and the limit of detection was 0.03 μg mL−1. The intra-day and inter-day accuracy were satisfactory, being in the range of 85.2 – 109.1 %. The robustness of the microextraction protocol was evaluated using DoE. The green potential and the practicality of the proposed analytical scheme were examined based on Green Analytical Procedure Index (GAPI) and Blue Applicability Grade Index (BAGI), respectively. A BAGI score of 65 was attained, demonstrating good applicability in terms of practicality, while the novel protocol was found to show green merits. The developed method can be used for the analysis of the drug in human urine.

Synthesis of novel MOF-on-MOF composite as a magnetic sorbent to dispersive micro solid phase extraction of benzodiazepine drugs prior to determination with HPLC-UV

Diazepam and lorazepam are two benzodiazepine drugs widely prescribed as antidepressants and antiepileptics. A straightforward and time-save dispersive micro solid phase extraction method as a sample preparation strategy was developed to extract these drugs in human urine and real water samples prior to their determination by HPLC-UV. A novel sorbent based on growing Co-MOF on Fe-MOF was synthesized and then magnetized using magnetic Fe3O4 nanoparticles and a sol–gel strategy. The sorbent (Fe3O4@SiO2@Co-MOF@Fe-MOF composite) showed the highest extraction efficiency toward diazepam and lorazepam compared to Fe-MOF and Co-MOF@Fe-MOF as sorbents. The effects of various factors on diazepam and lorazepam determination were studied by experimental design, in which a Plackett-Burman design and Box-Behnken design were used for screening the factors and optimizing the significant factors, respectively. Under optimum conditions, the method linearity for the diazepam and lorazepam determination was 0.3–450 and 0.2–400 ng mL−1 with an R2 of 0.9926 and 0.9943, respectively. Proper detection limits of 0.09 and 0.06 ng mL−1 were obtained for the diazepam and lorazepam determination. Also, intra-day and inter-day RSDs (n = 3) were in the range of 3.42–3.75 % and 4.76–5.39 % for the diazepam and lorazepam determination, respectively. The method exhibits a high preconcentration factor of 654.3 and 719.1 for the diazepam and lorazepam determination. Besides, the recoveries and RSDs were evaluated by analysis of tap, river, and well water, and two human urine samples using the method. RSDs were in the range of 3.09–6.80 %, with recoveries between 88.2 and 97.5 % for analysis of spiked real water and urine samples.

Green electrochemical methodology for simultaneous determination of atorvastatin and ezetimibe: Application to biological matrices

In this context, we report the first electrochemical sensing platform for the simultaneous quantitation of two antihyperlipidemic drugs, namely, atorvastatin (ATR) and ezetimibe (EZT), fabricated of manganese oxide nanoparticles/multi-walled carbon nanotubes/modified carbon paste electrodes (Mn2O3/MWCNT/MCPE). The developed composite was characterized physicochemical and electrochemically and the experimental conditions were optimized. Using square wave voltammetry (SWV), two wide linear dynamic ranges were attained for both drugs: 1.0–100 × 10−8 M and 2.0–100 × 10−6 M. The calculated detection and quantitation limits were 3.97 × 10−9 and 12.03 × 10−9 M for ATR and 4.66 × 10−9 and 14.12 × 10−9 M for EZT, respectively. The suggested platform was successfully applied for the simultaneous analysis of both drugs in human urine and plasma samples, in addition to a combined pharmaceutical dosage form (ATOZET® film coated tablets) and satisfactory percentage recoveries were obtained using Eco-scale and AGREE greenness tools for evaluating the greenness of analytical methodology.Furthermore, repeatability, stability testing, interferences study and greenness assessment were conducted and confirmed the reliability of the suggested platform for the simultaneous determination of both drugs in quality control laboratories.

Dried Urine Spot Analysis for assessing cardiovascular drugs exposure applicable in spaceflight conditions

Cardiovascular pharmacological countermeasures will be required as a preventive measure of cardiovascular deconditioning and early vascular ageing for long term space travelers. Physiological changes during spaceflight could have severe implications on drug pharmacokinetics and pharmacodynamics (PK/PD). However, limitations exist for the implementation of drug studies due to the requirements and constraints of this extreme environment. Therefore, we developed an easy sampling method on dried urine spot (DUS), for the simultaneous quantification of 5 antihypertensive drugs in human urine: irbesartan, valsartan, olmesartan, metoprolol and furosemide analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS), considering spaceflight parameters. This assay was validated in terms of linearity, accuracy, and precision with satisfactory results. There were no relevant carry-over, matrix interferences. The targeted drugs were stable in urine collected by DUS until 6 months at +21 °C, +4°C, −20 °C (with or without desiccants) and at 30 °C during 48 h. Irbesartan, valsartan and olmesartan were not stable at 50 °C during 48 h. This method was found to be eligible for space pharmacology studies in terms of practicality, safety, robustness and energy costs. It has been successfully implemented in space tests programs led in 2022.

Simultaneous determination of four sedative-hypnotics in human urine based on dendritic structured magnetic nanomaterials

A magnetic solid-phase extraction technique based on magnetic dendritic structured nanoparticles (Fe3O4@SiO2-NH2-G5) as adsorbent coupled with ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) has been developed to detect diazepam, midazolam, zolpidem, and zaleplon in human urine. With Fe3O4@SiO2-NH2 as the central core, dendrimer (G5) grafted alternately with cyanuric chloride and imidazole were bonded to the surface of the core to synthesize Fe3O4@SiO2-NH2-G5. The morphology and structure of the magnetic materials were characterized by transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and dynamic light scattering (DLS). The key parameters affecting the extraction efficiency were optimized. A satisfactory performance was obtained under the optimum extraction conditions. The proposed method was validated, and the limits of detection of zaleplon, diazepam, zolpidem, and midazolam were 0.05, 0.05, 0.02, and 0.02 ng mL−1, respectively. The linear correlation coefficients r of the four analytes were > 0.996, the intra-day precision was between 2.4 % and 9.4 % with the recoveries between 88.3 % and 104.8 %, and the inter-day precision ranged from 3.9 % to 15.2 % with the recovery in the range of 94.1 %−108.3 %. The magnetic dendritic structure nanomaterial Fe3O4@SiO2-NH2-G5 was successfully used to extract sedative-hypnotic drugs from human urine samples. The Fe3O4@SiO2-NH2-G5-based magnetic solid-phase extraction method eliminates centrifugation and filtration steps as in conventional extraction. Only one step of vortex dispersion extraction could achieve the separation and purification of the target compounds. The proposed method was simple, rapid, environment-friendly, and suitable for the analysis of sedative-hypnotic drugs in human urine.

Solvent bar microextraction combined with HPLC-DAD and multivariate optimization for simultaneous determination of three antiarrhythmic drugs in human urine and plasma samples

A sensitive and simple microextraction approach was developed and validated to simultaneously determine three antiarrhythmic drugs, propranolol, diltiazem, and verapamil, in human urine and plasma samples, by combining solvent bar microextraction (SBME) with high-performance-liquid- chromatography diode-array detection. The optimization of SBME was initially investigated following a full factorial design (FFD) and subsequently by central composite design (CCD). With only 27 extraction tests using CCD, the optimum extraction conditions for selected drugs by SBME methodology were determined. The CCD allowed examining the linear, interaction, and quadratic influence of factors on drugs’ extraction efficiencies% (EE%), resulting in reduced size of SBME experiments. Under the optimal conditions, the calibration curves were linear in the ranges of 1.73–103 / 2.56–103 μg L−1 for propranolol, 2.32–103/ 2.83–103 μg L−1 for diltiazem, and 4.54–103/ 5.97–103 μg L−1 for verapamil at the respective urine/ plasma samples with reasonable linearity R2 > 0.978 in both matrixes. The ranged value of intra precision (RSD%, n = 5) for the selected drugs were from 1.30 to 5.66 and from 3.00 to 7.80 in urine and plasma samples, respectively. The limits of detection in urine/ plasma were 0.52/ 0.77 μg L−1, 0.69/ 0.84 μg L−1, 1.36/ 1.79 μg L−1 for propranolol, diltiazem, and verapamil, respectively. In comparison with referenced methods and based on the satisfactory results of applications, the proposed method can be considered a potential method for biopharmaceutical analysis of selected antiarrhythmic drugs in biological samples.

Chemiluminescent Cucurbit[n]uril-Based Chemosensor for the Detection of Drugs in Biofluids.

Chemiluminescence-based detection methods offer a superior signal-to-noise ratio and are commonly adopted for biosensors. This work presents the design and implementation of a supramolecular assay based on a chemiluminescent chemosensor. Specifically, an indicator displacement assay (IDA) with the supramolecular host-guest complex of chemiluminescent phenoxy 1,2-dioxetane and cucurbit[8]uril enables the low-micromolar detection of drugs in human urine and human serum samples. Cucurbit[8]uril thereby acts as a non-surfactant chemiluminescence enhancer and a synthetic receptor. Additionally, we show that adding an equimolar amount of cucurbit[8]uril to a commercially available dioxetane used in standard enzymatic chemiluminescence immunoassays enhances the chemiluminescence by more than 15 times. Finally, we demonstrate that a chemiluminescence resonance energy transfer between a unimolecular macrocyclic cucurbit[7]uril-dye conjugate and a phenoxy 1,2-dioxetane can be utilized to detect the herbicide paraquat at a micromolar concentration in aqueous media.

Chemometric determination of common cold infection drugs in human urine

Abstract In this work, spectrophotometric identification of acetylsalicylic acid (ASA), paracetamol (PCM), and caffeine (CAF) (common cold infection drugs) in human urine samples was investigated. For ASA, PCM, and CAF, chemometric analysis of human urine samples has proved successful. Spectrophotometric analysis of common cold infection drugs was performed using multivariate calibration methods (principal component regression [PCR] and partial least-squares regression). For the simultaneous prediction of common cold infection drugs in prepared mixes and human urine samples without prior separation, two spectrophotometric-chemometric approaches were proposed. The synthetic mixes were made with common cold infection drugs in the first stage, and the absorbance values were obtained using spectrophotometry. The quantities of common cold infection drugs in the human urine sample were calculated in the second stage. The calibration curves for each medication are linear in the concentration range of the synthetic mixes. The two methods were tested for accuracy and repeatability, and high recoveries and low standard deviations were calculated. sum of prediction residual errors, observation limit, and detection limit, and % recovery values, which are the analytical properties of the proposed methods, were 0.00029, 0.096, and 0.290, respectively; 0.0069, 0.086, and 0.260; 0.0077, 0.094, and 0.285; 0.0049, 0.066, and 0.199 for PCM, ASA, and CAF for the principal component regression method, respectively; 0.0059, 0.066, and 0.199; 0.0065, 0.069, and 0.210. The results produced using the employed chemometric methods are quick, easy, and consistent. The proposed methods are extremely sensitive and precise and have thus been effectively employed to detect active chemicals (ASA, PCM, and CAF) in human urine samples.

Rapid On-Site Detection of Various Amphetamine-Type Drugs in Human Urine and Hair by Portable Pulsed Direct Current Electrospray Ionization Mass Spectrometry

Rapid On-Site Detection of Various Amphetamine-Type Drugs in Human Urine and Hair by Portable Pulsed Direct Current Electrospray Ionization Mass Spectrometry

Combination of fabric phase sorptive extraction with UHPLC-ESI-MS/MS for the determination of adamantine analogues in human urine

Herein, fabric phase sorptive extraction – a member of sorbent-based microextraction family – is utilized for the rapid isolation of selected antiviral drugs namely amantadine, memantine and rimantadine from human urine prior to their analysis with UHPLC-MS/MS. Fabric phase sorptive extraction membrane coated with sol–gel sorbent coated poly(propylene glycol)-poly(ethylene glycol)-poly(propylene glycol) sorbent was identified as the optimum extraction membrane for the target analytes. Due to the engineered affinity of the fabric phase sorptive extraction towards the analytes, the extraction proceeds in relatively short time (20 min) while its high permeability permits the extraction of biological samples without any other pretreatment. Following selection of the appropriate membrane, significant parameters including extraction time, sample volume, membrane size, elution solvent, etc were optimized. The drugs were analyzed under positive electrospray ionization using multi-reaction monitoring mode. The method was linear in the range of 5 – 100 ng mL−1 by constructing weighted matrix-matched calibration curves. The intra-day and inter-day accuracy were ranged between – 18.7 to + 18.1% and – 18.3 to + 16.1%, respectively. The precision of the method (intra-day, inter-day) were less than 18.5 % in all cases. The method limits of detection were in the range of 0.2 – 0.8 ng mL−1 while the lower limit of quantitation was set at 5 ng mL−1 for all analytes. The developed analytical scheme was efficiently applied to the analysis of the target drugs in human urine and could be adopted as a rapid and robust green analytical tool for clinical applications.

Salting-out homogeneous liquid-liquid microextraction for the determination of azole drugs in human urine: Validation using total error concept.

A salting-out homogeneous liquid-liquid microextraction was proposed for the quantification of four azole drugs in human urine prior to high-performance liquid chromatography analysis. The procedure involved the mixing of the sample with acetonitrile in appropriate volumes followed by the addition of sodium sulfate solution in order to facilitate phase separation. The parameters influencing the extraction performance were studied and optimized using a two-step experimental design. The analytical procedure was thoroughly validated using the accuracy profiles as a graphical decision-making tool. The β-expectation tolerance intervals did not exceed the acceptance criteria of ±15% meaning that 95% of future results will be included in the defined bias limits. The limits of detection of the procedure were satisfactory, ranging between 0.01 and 0.03 μg/mL. The mean analytical bias in the spiking levels was satisfactory and ranged between -10.3 and 4.2% while the relative standard deviation was lower than 5.6%. Monte-Carlo simulations followed by capability analysis were employed to investigate the ruggedness of the sample preparation protocol. The developed method offers advantages compared to previously reported approaches for the same type of analysis including extraction efficiency and scaling down of the sample volume and extraction time.

Development of a chemosensor probe based on functionalised poly[β-(1→4)-2-amino-2-deoxy-D-glucopyranose]-cobalt nanoparticles for the selective detection of flunitrazepam

ABSTRACT Flunitrazepam abuse as ‘date-rape’ drug is on the increase. A colorimetric probe was developed by grafting cobalt nanoparticles (CoNPs) onto poly[β-(1→4)-2-amino-2-deoxy-D-glucopyranose] functionalized thymol blue (CFTB) backbone for the detection of flunitrazepam drug in human urine (ex-situ). Studies revealed an interaction between CFTB and Co with the formation of a five-membered ring chelated compound (FTIR), while high thermal stability properties were displayed by CFTB-CoNPs without any change in the composition of the material (TGA). The distribution of CoNPs showed an irregular spherical pore deposited on the surface of CFTB (SEM) in the dimension of 100 nm (TEM). The interaction between the CFTB-CoNPs probe and the flunitrazepam was due to ionic bonding between the protonated amine group in the biopolymer and the fluoro group of flunitrazepam. The highly selective and sensitive CFTB-CoNPs probe was able to detect at 1.00µg/L with an instant and distinct colour change from wine to orange.

Rapid simultaneous clinical monitoring of five oral anti-coagulant drugs in human urine using green microextraction technique coupled with LC–MS/MS

ObjectivesThere is no analytical method for simultaneous monitoring of warfarin and novel direct oral anticoagulants (NOACs) in human urine samples in a single run in the clinics. Although several studies have reported their measurements in human blood samples, but its sample collection is more invasive and time-consuming, thereby challenging to monitor frequently. MethodsIn this work, we developed a fast microextraction technique (ultrasound-assisted salt-induced liquid-liquid microextraction, USA-SI-LLME) coupled with high-performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS) to rapidly quantify four commonly used NOACs drugs (apixaban, dabigatran, edoxaban, and rivaroxaban) and warfarin in human urine samples. USA-SI-LLME conditions were optimized using a water-miscible organic solvent as an extraction solvent, high salt concentrations, sample pH, and extraction time (∼5.5 min). Results and conclusionsThe analytical method showed excellent linearities from 0.5 to 500 μg/L for apixaban, edoxaban, rivaroxaban, warfarin, and 1 ∼ 500 μg/L for dabigatran. Intra- and inter-day precision values were <9.31% and R2 > 0.99 for all analytes. Limits of detection ranged between 0.07 ∼ 0.18 μg/L, and relative recoveries ranged between 92.18 and 110.15%. This method was successfully applied to analyze 15 one-spot urine samples from 15 clinical patients who regularly took warfarin or NOACs, and high accuracy was found. We concluded that this method could be used as a non-invasive high-throughput and rapid monitoring of NOACs and warfarin in human urine in clinical settings and could provide timely analysis during emergency care.

A Dilute-and-Shoot LC-MS/MS Method for Screening of 43 Cardiovascular Drugs in Human Urine

A simple, specific, and economical LC-MS/MS method was investigated for the screening of 43 prescribed antihypertensive and related drugs in human urine. The urine samples were simply prepared by diluting and mixing with internal standard before directly introduced to the LC-MS/MS system, which is fast, straightforward, and cost-effective. Fractional factorial, Box-Behnken, and I-optimal design were applied to screen and optimize the mass spectrometric and chromatographic factors. The analysis was carried out on a triple quadrupole mass spectrometer system utilizing multiple reaction monitoring with positive and negative electrospray ionization method. Chromatographic separation was performed on a Thermo Scientific Accucore RP-MS column (50 × 3.0 mm ID., 2.6 μm) using two separate gradient elution programs established with the same mobile phases. Chromatographic separation was performed within 12 min. The optimal method was validated based on FDA guideline. The results indicated that the assay was specific, reproducible, and sensitive with the limit of detection from 0.1 to 50.0 μg/L. The method was linear for all analytes with coefficient of determination ranging from 0.9870 to 0.9981. The intra-assay precision was from 1.44 to 19.87% and the inter-assay precision was between 2.69 and 18.54% with the recovery rate ranges from 84.54 to 119.78% for all drugs measured. All analytes in urine samples were stable for 24 h at 25℃, and for 2 weeks at -60℃. The developed method improves on currently existing methods by including larger number of cardiovascular medications and better sensitivity of 12 analytes.

Discrimination of narcotic drugs in human urine based on nanoplasmonics combined with chemometric method

The detection of psychoactive substances is an important branch of modern analytical chemistry and has many legally and socially relevant implications. The use of a surface plasmon resonance (SPR)-based gene–nanoparticle system has emerged as a promising technique for the rapid and ultrasensitive detection of molecular species such as drugs of abuse in biofluids. However, the development of a viable screening tool for the detection of multiple classes of drugs in complex media is a considerable challenge because the existing techniques lack affinity toward certain species due to matrix interference. Our aim was to develop a simple optical sensor array for the classification of nine narcotic drugs in aqueous solution and human urine. The UV–vis spectra of DNA–gold nanoparticles in the presence of nine narcotic drugs (pentobarbital sodium, caffeine, morphine, remifentanil, fentanyl, ketamine, etomidate, carfentanil, and sulfentanyl) were distinctly different. Furthermore, the narcotic drugs present in aqueous solution and in human urine were classified correctly through partial least squares discriminant analysis (PLS-DA). Combination with a multi-sensor unit further improved the prediction accuracy of the PLS-DA models. The proposed method has potential for on-site drug detection and drug abuse screening.

On-chip ion pair-based dispersive liquid-liquid extraction for quantitative determination of histamine H2 receptor antagonist drugs in human urine

In the present work, an ion-pair based dispersive liquid-liquid microextraction was performed on a centrifugal chip for the first time. The entire DLLME procedure, including flow direction, desperation, and sedimentation of the extracting phase, can be fulfilled automatically on a solitary chip. The chip was made of Poly(methyl methacrylate) (PMMA) and was of two units for two parallel extractions, each consisting of three chambers (for the sample solution, extracting solvents, and sedimentation). As the chip rotated, fluids flowed within the chip, and the dispersion, mixing, extraction, and sedimentation of the final phase were performed on the chip by simply adjusting the spin speed. Determination of two histamine H2 receptor antagonist drugs, cimetidine and ranitidine, as the model analytes from the urine samples was done using the developed on-chip ion-pair based DLLME method followed by an HPLC-UV. The effective parameters on the extraction efficiency of the model analytes were investigated and optimized using the one variable at a time method. Under optimized conditions, the calibration curve was linear in the range of 15–2000 μg L−1 with a coefficient of determination (R2) more than 0.9987. The relative standard deviations (RSD %) for extraction and determination of the analytes were less than 3.7% based on five replicated measurements. LODs less than 10.0 μg L−1 and preconcentration factors higher than 39-fold were obtained for both of the model analytes. The proposed chip enjoys the advantages of both the DLLME method and miniaturization on a centrifugal chip.

The Determination of Parkinson's Drugs in Human Urine by Applying Chemometric Methods.

The spectrophotometric-chemometric analysis of levodopa and carbidopa that are used for Parkinson's disease was analyzed without any prior reservation. Parkinson's drugs in the urine sample of a healthy person (never used drugs in his life) were analyzed at the same time spectrophotometrically. The chemometric methods used were partial least squares regression (PLS) and principal component regression (PCR). PLS and PCR were successfully applied as chemometric determination of levodopa and carbidopa in human urine samples. A concentration set including binary mixtures of levodopa and carbidopa in 15 different combinations was randomly prepared in acetate buffer (pH 3.5).). UV spectrophotometry is a relatively inexpensive, reliable, and less time-consuming method. Minitab program was used for absorbance and concentration values. The normalization values for each active substance were good (r2>0.9997). Additionally, experimental data were validated statistically. The results of the analyses of the results revealed high recoveries and low standard deviations. Hence, the results encouraged us to apply the method to drug analysis. The proposed methods are highly sensitive and precise, and therefore they were implemented for the determination of the active substances in the urine sample of a healthy person in triumph.