Analysis Of Non-steroidal Anti-inflammatory Drugs Research Articles

Quantitative analysis of nonsteroidal anti-inflammatory drugs in dried blood spot from mountain ultra-trail runners. Contribution of pharmacokinetic models for the interpretation of the results.

Monitoring of drug use in athletes is of interest both for health and competition-related issues. Considering the advantages of Dried Blood Sampling (low invasiveness, easy sampling, long term storage), we have validated a quantitative LC-MS/HRMS method for the screening of 16 nonsteroidal anti-inflammatory drugs. For all drugs, accuracy and imprecision were within 15% for the 3 levels of quality control and lower than 20% for the lower limit of quantification. Application was performed from samples obtained for Ultra-Trail du Mont-Blanc® 2021 and 2022. A focus on ibuprofen and its metabolites (hydroxyibuprofen, carboxyibuprofen, ibuprofen glucuronide and hydroxyibuprofen glucuronide) was made because the results showed that it was the most detected nonsteroidal anti-inflammatory drug. Further, an interpretation of the ibuprofen concentrations was proposed either from experimental data obtained after an intake of ibuprofen by 10 control subjects, or from a pharmacokinetic modelling and simulations. Depending on the analytical performances of the method, we proposed possible detection windows for ibuprofen in runners. The pharmacokinetic model made it possible to consider two scenarios with and without modification of the total clearance of ibuprofen linked to a modification of the pharmacokinetics of the drugs due to the practice of a long and intense physical activity.

A mixed-mode reversed-phase/strong-anion-exchange stationary phase: Analyte-retention stability and application in the analysis of nonsteroidal anti-inflammatory drugs

Mixed-mode reversed-phase/anion-exchange chromatography (RP/AEX) is an effective method for the chromatographic analysis of acidic drugs because it combines reversed-phase chromatography (RP) with anion-exchange chromatography (AEX). However, the result repeatability for the RP/AEX analysis of acidic drugs is frequently compromised by the detrimental effects of residual silanol groups in an RP/AEX stationary phase on peak separation and analyte retention. In this study, an RP/weak-AEX stationary phase with amino anion-exchange groups, Sil-AA, was prepared. Subsequently, an RP/strong-AEX stationary phase, Sil-PBQA, was prepared by replacing the amino groups in Sil-AA with a benzene ring and a benzyl-containing quaternary ammonium salt. The chromatographic behaviors of Sil-PBQA and Sil-AA were compared, and the effect of residual silanol groups on the chromatographic behavior of an RP/AEX stationary phase was evaluated. Residual silanol groups not only caused additional electrostatic interactions for acidic analytes, but also competed with the analytes for the anion-exchange sites in an RP/AEX stationary phase. The effects of different salt-containing mobile-phase systems on the analyte-retention behavior of Sil-PBQA were investigated to develop a method that enhanced the repeatability of the RP/AEX acidic-analyte-analysis results obtained using Sil-PBQA and facilitated the separation of nonsteroidal anti-inflammatory drugs on Sil-PBQA. The ideas presented in this paper can improve the separation of peaks and repeatability of results in the RP/AEX analysis of acidic drugs.

Emerging Developments in Separation Techniques and Analysis of Chiral Pharmaceuticals.

Chiral separation, the process of isolating enantiomers from a racemic mixture, holds paramount importance in diverse scientific disciplines. Using chiral separation methods like chromatography and electrophoresis, enantiomers can be isolated and characterized. This study emphasizes the significance of chiral separation in drug development, quality control, environmental analysis, and chemical synthesis, facilitating improved therapeutic outcomes, regulatory compliance, and enhanced industrial processes. Capillary electrophoresis (CE) has emerged as a powerful technique for the analysis of chiral drugs. This review also highlights the significance of CE in chiral drug analysis, emphasizing its high separation efficiency, rapid analysis times, and compatibility with other detection techniques. High-performance liquid chromatography (HPLC) has become a vital technique for chiral drugs analysis. Through the utilization of a chiral stationary phase, HPLC separates enantiomers based on their differential interactions, allowing for the quantification of individual enantiomeric concentrations. This study also emphasizes the significance of HPLC in chiral drug analysis, highlighting its excellent resolution, sensitivity, and applicability. The resolution and enantiomeric analysis of nonsteroidal anti-inflammatory drugs (NSAIDs) hold great importance due to their chiral nature and potential variations in pharmacological effects. Several studies have emphasized the significance of resolving and analyzing the enantiomers of NSAIDs. Enantiomeric analysis provides critical insights into the pharmacokinetics, pharmacodynamics, and potential interactions of NSAIDs, aiding in drug design, optimization, and personalized medicine for improved therapeutic outcomes and patient safety. Microfluidics systems have revolutionized chiral separation, offering miniaturization, precise fluid control, and high throughput. Integration of microscale channels and techniques provides a promising platform for on-chip chiral analysis in pharmaceuticals and analytical chemistry. Their applications in techniques such as high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) offer improved resolution and faster analysis times, making them valuable tools for enantiomeric analysis in pharmaceutical, environmental, and biomedical research.

A journey of 10 years in analytical method development and environmental monitoring of pharmaceuticals in South African waters

Apart from the studies which reported the occurrence of steroid hormones and antibiotics in wastewater treatment plants (WWTPs) back in 2004, 2007 and 2012, the evidence for monitoring of pharmaceuticals in South African water bodies intensified from 2014. Therefore, this study reviewed the analytical methods developed and applied in South Africa for the purpose of monitoring pharmaceuticals and their metabolites in water. At the same time, pharmaceuticals and their metabolites detected in South African waters are reviewed. To date, there is over 100 pharmaceuticals detected in South African waters with most studies focussing on quantitative analysis of non-steroidal anti-inflammatory drugs (NSAID), antibiotics, antiretroviral drugs and carbamazepine. Various sources of pharmaceuticals in the environment are reported, with WWTPs found as the major contributor to their occurrence in South African rivers. Notably, a NSAID, ibuprofen, with concentrations found exceeding 100 μg L-1 in selected WWTPs has also been found at high levels reaching 60 μg L-1 in river water. Mostly, pharmaceuticals detected in wastewater are also reported in corresponding rivers. The present review details pharmaceuticals that should be included in environmental monitoring studies performed in South Africa, while also identifying areas for future research through the research gap analysis.

Ultra fast liquid chromatographic analysis of nonsteroidal anti-inflammatory drugs with fluorimetric detection in tap water, urine, and pharmaceutical samples

ABSTRACT A novel analytical method based on ultra-fast liquid chromatography using fluorimetric detector was developed and validated for determination of non-steroidal anti-inflammatory drugs (NSAIDs) (ibuprofen (IBP), etodolac (ETD), dexketoprofen (DKP), sodium diclofenac (SDCF), and naproxen (NPX) in tap water, urine and pharmaceutical samples. Precolumn derivatisation of targeted NSAIDs was carried out with 4-bromomethyl-7-methoxy coumarin (BrMmC) using dibenzo-18-crown-6-ether as reaction catalyst leading to the formation of a fluorescent compound. The obtained fluorescent compound of NSAIDs were measured at excitation wavelength as 325 nm, and emission wavelength of 395 nm. Optimum analytical conditions were carefully studied and improved. C18 column, with the dimensions of 4.0 × 100 mm and 3 µm particle size, was used. Gradient elution with methanol: water 40:60; v/v (eluent A) and acetonitrile 100% (eluent B) were used as mobile phase and flow rate of 0.4 mL/min. The linearity range of the analytes were between 0.01–10.0 µg mL−1. Recovery values obtained from pharmaceutical preparations were found as 100.04%, 99.99%, 100.09%, 99.98% and 100.47% for IBP, ETO, DKP, SDCF, NPX, respectively. LOD values were found to vary between 0.00009 µg mL−1 and 0.00048 µg mL−1 in tap water, urine and pharmaceutical samples. The optimised technique was successfully applied for the determination of NSAIDs in tap water, urine, and pharmaceutical specimen. The specified NSAIDs were not found in real tap water samples.

Introduction of a Zn-based metal\u2013organic framework @ biomass porous activated carbon as a high-sensitive coating for a stainless steel SPME fiber: application to the simultaneous analysis of nonsteroidal anti-inflammatory drugs

The present study introduces a high-efficiency nanocomposite material featuring a zinc-based metal–organic framework and a novel porous activated carbon derived from bread waste. The prepared nanocomposite, namely Zn-MOF-5@BHPAC, has been synthesized by a low-temperature hydrothermal process and coated onto the surface of a stainless steel wire with epoxy glue. The fabricated fiber has been employed as an SPME fiber applied in the extraction and pre-concentration of some nonsteroidal anti-inflammatory drugs (NSAIDs) before their high-performance liquid chromatography-ultraviolet (HPLC-UV) studies. The characterization studies were performed utilizing field emission scanning electron microscopy, elemental mapping, energy-dispersive X-ray spectroscopy, elemental analyzer, Fourier-transform infrared spectroscopy, and Brunauer–Emmett–Teller surface area analysis. Under the optimal conditions, the method demonstrated low detection limits (LODs, 0.06–0.15 µg L–1), wide linear ranges (LRs, 0.20–380 µg L–1) with good linearity (R2 > 0.991), good precisions (RSDs < 6.95%), and acceptable relative recoveries (RR > 85%). Using the green and affordable biomass of bread as a novel carbon-rich source is an innovative idea provided in this study. In addition, the hybridization of the obtained carbon-based material with the MOF compound to create a new high-capacity sorbent is another strength of the proposed method. Long service lifetime, economic efficiency, environmental friendliness, and high extraction capability were some of the other advantages of the suggested procedure. Therefore, the method can utilize successfully for the simultaneous determination of NSAIDs (as model analytes) in different matrixes.

Multi-template molecularly imprinted polymer hybrid nanoparticles for selective analysis of nonsteroidal anti-inflammatory drugs and analgesics in biological and pharmaceutical samples.

The multi-template molecularly imprinted polymers reinforced with hybrid oxide nanoparticles were developed for the selective separation and determination of the trace level of naproxen (NPX), methocarbamol (MTH), and omeprazole (OMZ) simultaneously from biological and pharmaceutical samples. The polymers were constructed by magnetic core@shell molecularly imprinted polymer nanocomposite (Fe3O4/ZnO/CuO/MWCNT@MIP). An electrochemical sensor has been fabricated for this purpose. Fe3O4/ZnO/CuO/MWCNT nanocomposite was introduced to improve the electron transport capability and increase the sensor surface area, as well as enhance the electronic conductivity. The triple-template MIP-coated layer provides simultaneous selective identification of three analytes by using [Fe (CN)6]3-/4-as the redox probe. Electrochemical behavior of MTH, NPX, and OMZ on the modified electrode (Fe3O4/ZnO/CuO/MWCNT@MIP) by various techniques such as cyclic voltammetry, differential pulse voltammetry, and chronoamperometry was examined. The morphology of the modified and unmodified carbon paste electrodes was performed by scanning electron microscopy (SEM) and X-ray diffraction analysis (XRD). The average crystal size for fabricated nanoparticles obtained by calculating the X-ray diffraction technique was 17nm in the Scherer method. The particle size which was determined by SEM was 48nm. Some electrochemical parameters such as the diffusion coefficient and electron transfer coefficient were determined. The effect of many variables such as the pH and scan rate was also investigated. Under optimal conditions, the sensor is designed in the linear range 5.0nM-100μM and 5.0nM-100μM and 1.0nM-130μM with a detection limit of 1.5nM, 1.0nM, and 0.7nM for measurement OMZ, NPX, and MTH, respectively. The relative standard deviation (RSD) of the five measurements was 1.21%, 2.23%, and 2.56% for NPX, MTH, and OMZ. Finally, the designed sensor was successfully used for simultaneous detection of target analytes in the real samples; tablets, water samples, and biological samples.

Measuring the mass of an electron: an undergraduate laboratory experiment with high resolution mass spectrometry

Abstract High-resolution mass spectrometry (HRMS) has become increasingly affordable and user-friendly. Its potential spans a wide range of applications and experiments including the measurement of accurate masses, supporting the elucidation of elemental compositions and the identification of unknown compounds. To illustrate the main features of mass spectrometry, and particularly, of HRMS, we have designed and implemented a 3-h laboratory experiment using direct infusion electrospray HRMS analysis of non-steroidal anti-inflammatory drugs (e.g., ibuprofen or naproxen) solutions, acquiring full-scan spectra in both positive and negative ionization modes. The experimental accurate mass measurements (m/z values) of selected characteristic fragment ions -so called twin ions, with common elemental composition in both ionization modes but with different charge, allow the indirect measurement of the mass of an electron with relative errors below 5% with respect to the accepted IUPAC value (0.00055 Da). The experiment demonstrates how powerful and useful HRMS can be for research challenges often encountered during undergraduate or graduate research projects as well as for addressing undergraduate level general chemistry problems that provide the opportunity to discuss aspects related to the Nature of Science in an analytical chemistry context (such as measurement precision and accuracy).

Ultrasonic assisted magnetic solid phase extraction based on the use of magnetic waste-tyre derived activated carbon modified with methyltrioctylammonium chloride adsorbent for the preconcentration and analysis of non-steroidal anti-inflammatory drugs in wastewater

In this study, a magnetic waste-tyre derived activated carbon modified with methyltrioctylammonium chloride, was successfully synthesized, characterised, and applied for the extraction and preconcentration of four non-steroidal anti-inflammatory drugs in wastewater. The scanning electron microscopy and N 2 -adsorption/desorption analysis results confirmed that the synthesized nanocomposite was porous with a large specific surface area of 570 m 2 g −1 . The significant factors affecting the Ultrasonic assisted magnetic solid phase extraction method were investigated using univariate approach and response surface methodology. The optimum conditions for the extraction and preconcentration of the target analytes were 0%, 15 min, 6.5 and 30 mg, for ionic strength, extraction time, pH and adsorbent mass respectively. The quantification of the target analytes was performed using high performance liquid chromatography equipped with diode array detector. Under optimum conditions, low limits of detection and quantification ranging between 0.054–0.38 μg L −1 and 0.18–1.27 μg L −1 , respectively, were obtained. A wide linearity (ranging from limit of detection – 500 μg L −1 with R 2 ≥ 0.99) and precision lower than 7%, were achieved. The applicability of proposed method was evaluated for the determination of naproxen, ketoprofen and diclofenac in wastewater.

Analysis of Nonsteroidal Anti-inflammatory Drugs by using Microfluidic Techniques: A Review

In this review paper, miniaturized techniques, including both electromigration and liquid chromatographic techniques, have been discussed considering their main features in the analytical field for the separation and analysis of Nonsteroidal Anti-inflammatory Drugs (NSAIDs). In Capillary Electrophoresis (CE) and nano-liquid chromatography (nano-LC), separation is performed in capillaries with Internal Diameter (I.D.) lower than 100 μm and therefore flow rates in the range 100-1000 nL/min are applied. Therefore, due to the low flow rate, high mass sensitivity can be obtained. Usually, conventional UV detectors are used on-line; however, these techniques can be coupled with Mass Spectrometry (MS). CE and nano-LC have also been applied to the separation of NSAIDs using silica stationary phases (SP) modified with C&lt;sub&gt;18&lt;/sub&gt; promoting interaction with analytes mainly based on hydrophobic interaction. Besides, the use of chiral SP was found to be effective for the chiral resolution of these compounds. In addition to silica phases, monolithic (both organic and inorganic) material has also been used. Although most of the presented studies aimed to demonstrate the usefulness of the considered microfluidic techniques, some applications to real samples have also been reported.

Exploratory Genome-Wide Interaction Analysis of Nonsteroidal Anti-inflammatory Drugs and Predicted Gene Expression on Colorectal Cancer Risk.

Regular use of nonsteroidal anti-inflammatory drugs (NSAID) is associated with lower risk of colorectal cancer. Genome-wide interaction analysis on single variants (G × E) has identified several SNPs that may interact with NSAIDs to confer colorectal cancer risk, but variations in gene expression levels may also modify the effect of NSAID use. Therefore, we tested interactions between NSAID use and predicted gene expression levels in relation to colorectal cancer risk. Genetically predicted gene expressions were tested for interaction with NSAID use on colorectal cancer risk among 19,258 colorectal cancer cases and 18,597 controls from 21 observational studies. A Mixed Score Test for Interactions (MiSTi) approach was used to jointly assess G × E effects which are modeled via fixed interaction effects of the weighted burden within each gene set (burden) and residual G × E effects (variance). A false discovery rate (FDR) at 0.2 was applied to correct for multiple testing. Among the 4,840 genes tested, genetically predicted expression levels of four genes modified the effect of any NSAID use on colorectal cancer risk, including DPP10 (PG×E = 1.96 × 10-4), KRT16 (PG×E = 2.3 × 10-4), CD14 (PG×E = 9.38 × 10-4), and CYP27A1 (PG×E = 1.44 × 10-3). There was a significant interaction between expression level of RP11-89N17 and regular use of aspirin only on colorectal cancer risk (PG×E = 3.23 × 10-5). No interactions were observed between predicted gene expression and nonaspirin NSAID use at FDR < 0.2. By incorporating functional information, we discovered several novel genes that interacted with NSAID use. These findings provide preliminary support that could help understand the chemopreventive mechanisms of NSAIDs on colorectal cancer.

A Zr-MOF@GO-Coated Fiber with High Specific Surface Areas for Efficient, Green, Long-Life Solid-Phase Microextraction of Nonsteroidal Anti-inflammatory Drugs in Water

A composite material featuring a zirconium-based metal–organic framework and graphene oxide (Zr-MOF@GO) was synthesized by a hydrothermal method and bonded to a stainless steel wire with an inorganic binder as a solid-phase microextraction (SPME) fiber for the derivatization-free extraction and analysis of nonsteroidal anti-inflammatory drugs (NSAIDs) coupled with gas chromatography (GC). The force between the Zr-MOF@GO and NSAIDs includes coordination action, H-bonding, and π–πconjugation effect, which results in the better extraction performance than a commercial polyamide fiber. The developed method achieved low detection limits (0.001–0.030 µg L−1, S/N = 3) and wide linear range (0.01–500 µg L−1) with good linearity (R ≥ 0.9970). The fiber coating had a high scratch resistance, which could effectively prevent coating wear and failure due to the friction between the fiber and the casing. Combined with the high thermal and chemical stability, the loss-free service life of the coating reached at least 240 extractions. Particularly, the derivatization-free extraction technique can greatly reduce the extraction time and use of organic solvents, thus maximizing the SPME technology advantages. It is evident that the analysis method is simple, environmentally friendly, and fast for detecting NSAIDs in water with high efficiency and long service life.

Optimization and application of hollow fiber liquid-phase microextraction and microwave-assisted extraction for the analysis of non-steroidal anti-inflammatory drugs in aqueous and plant samples.

Human consumption of non-steroidal anti-inflammatory drugs (NSAIDs) is increasing, which poses a great risk of pollution by these pharmaceuticals on the aquatic environment. Therefore, this study reports the optimization of microwave-assisted extraction using water as a green solvent and hollow fiber liquid-phase microextraction (HF-LPME) methods followed by high-performance liquid chromatography-high resolution mass spectrometry analysis of NSAIDs in wastewater and aquatic plant, Eichhornia crassipes. The optimized MAE resulted in efficient transfer of selected NSAIDs from plant samples into the aqueous phase yielding the recoveries ranging from 91 to115%. A multivariate approach based on half fractional factorial and central composite design was used during the optimization of HF-LPME. Under the optimized conditions, the maximum enrichment factors for naproxen, fenoprofen, diclofenac, and ibuprofen were 49, 126, 93 and 156, respectively. The overall analytical method recoveries ranged from 86 to 116% while the limits of quantitation for wastewater and plant samples ranged from 0.09 to 0.59μgL-1 and from 0.11 to 0.59μgkg-1, respectively. The precision of the proposed analytical method which was measured in terms of RSD values did not exceed 5%. Naproxen was the most abundant compound in both wastewater and the Eichhornia crassipes plant samples with concentrations of up to 3.30μgL-1 and 10.97μgkg-1, respectively. The detection of NSAIDs in Eichhornia crassipes means this plant has the ability to bioaccumulate pharmaceutical load in surface water.

Application of Molecularly Imprinted Polymers (MIP) and Flowing Atmospheric-Pressure Afterglow Mass Spectrometry (FAPA-MS) to Analysis of Nonsteroidal Anti-Inflammatory Drugs (NSAIDs)

In recent years, the rapid development of the pharmaceutical industry and the extensive and illicit use of painkillers have led to increased levels of nonsteroidal anti-inflammatory drugs (NSAIDs) in the environment. In view of the significant impact of NSAIDs on living organisms, including humans, their presence in the environment needs to be continuously monitored at trace levels. For this purpose, a combination of molecularly imprinted solid-phase extraction (MISPE) and HPLC-MS analysis is commonly used. MISPE has been utilized in direct, fast, and ecological analysis of drugs using a flowing atmospheric-pressure afterglow ion source for mass spectrometry (FAPA-MS). The new method was applied herein in the determination of naproxen, diclofenac, and ibuprofen. The linear dependence of the intensity of analytical signals on the amount of drugs is in the range of 0.2 μg to 1 g and the method detection limit (MDL) for all drugs is 0.2 μg in environmental samples. The new method also decreased the number of analytical stages, the time and cost of analysis, and the organic solvent consumption, besides being environmentally friendly.

Cotton thread modified with ionic liquid copolymerized polymer for online in-tube solid-phase microextraction and HPLC analysis of nonsteroidal anti-inflammatory drugs.

Cotton fiber is a biodegradable material that possesses properties such as high specific area, adjustable shape, and hygroscopicity. In this work, organic polymer was directly in situ grown on the surface of cotton thread and packed into a poly(ether ether ketone) tube for online in-tube solid-phase microextraction. The novel strategy solves the problems like high backpressure and tedious optimization process of normal monolithic polymer-based in-tube solid-phase microextraction capillary. The quaternary ammonium typed ionic liquid of 1-allyl-methylimidazolium chloride, 4-vinylbiphenyl, and ethylene dimethacrylate were co-polymerized and in situ grown on the surface of cotton thread as extraction phase. The solid-phase microextraction tube showed excellent performance for the extraction of three nonsteroidal anti-inflammatory drugs including ketoprofen, naproxen, and flurbiprofen due to the strong ion exchange and hydrophobic interactions. After online coupling with a high-performance liquid chromatography system by six-port valve, the method was applied for the quantitative analysis of nonsteroidal anti-inflammatory drugs in human plasma samples showing good enrichment performance (enrichment factor between 263 and 279), high sensitivity, good linearity, and good reproducibility.

Ultrasonic Followed by Solid Phase Extraction and Liquid Chromatography-Photodiode Array for Determination of Pharmaceutical Compounds in Sediment and Soil.

This work reports on the method optimization and application for quantitative analysis of non-steroidal anti-inflammatory drugs and anti-epileptic drug in soil and sediment samples. The analytes were extracted by ultrasonic extraction followed by solid phase extraction and quantified using liquid chromatographic coupled with photodiode array. The sensitivity of the method was determined based on the limit of detection and the limit of quantification which ranged between (0.010-0.027µg/kg) and (0.025-0.049µg/kg), respectively. The %recoveries of the method ranged between 74% and 112%. The concentrations obtained in real samples ranged from 0.055 to 0.426µg/kg in sediment and 0.044-0.567µg/kg in soil samples. The highest concentration was found for diclofenac in soil samples.

Efficacy and safety of anti-inflammatory agents for the treatment of major depressive disorder: a systematic review and meta-analysis of randomised controlled trials

ObjectivesTo systematically review the efficacy and safety of anti-inflammatory agents for patients with major depressive disorders.MethodsWe searched the literature to identify potentially relevant randomised controlled trials (RCTs) up to 1...

Using a Molecular Sensor Array with Colorimetric Detection to Identify Active Ingredients in Drug Formulations

A method for multiplex digital colorimetric qualitative analysis of nonsteroidal anti-inflammatory drugs (meloxicam, acetylsalicylic acid and its metabolites, paracetamol), β-adrenoblockers (carvedilol), secretolytics (bromhexine), fluoroquinolones (ofloxacin), metabolic stimulants (meldonium dihydrate), etc., was developed. The molecular chip operating efficiency was confirmed by verifying the authenticity of >40 medicinal substances. The proposed universal approach was new in principle and could be used for pharmaceutical quality control.

Multi-walled Carbon Nanotubes Reinforced into Hollow Fiber by Chitosan Sol-gel for Solid/Liquid Phase Microextraction of NSAIDs from Urine Prior to HPLC-DAD Analysis.

The efficient analytical method for the analysis of nonsteroidal antiinflammatory drugs (NSAIDs) in a biological fluid is important for determining the toxicological aspects of such long-term used therapies. In the present work, multi-walled carbon nanotubes reinforced into a hollow fiber by chitosan sol-gel assisted-solid/ liquid phase microextraction (MWCNTs-HF-CA-SPME) method followed by the high-performance liquid chromatography-diode array detection (HPLC-DAD) was developed for the determination of three NSAIDs, ketoprofen, diclofenac, and ibuprofen in human urine samples. MWCNTs with various dimensions were characterized by various analytical techniques. The extraction device was prepared by immobilizing the MWCNTs in the pores of 2.5 cm microtube via chitosan sol-gel assisted technology while the lumen of the microtube was filled with few microliters of 1-octanol with two ends sealed. The extraction device was operated by direct immersion in the sample solution. The main factors influencing the extraction efficiency of the selected NSAIDs have been examined. The method showed good linearity R2 ≥ 0.997 with RSDs from 1.1 to 12.3%. The limits of detection (LODs) were 2.633, 2.035 and 2.386 µg L-1, for ketoprofen, diclofenac, and ibuprofen, respectively. The developed method demonstrated a satisfactory result for the determination of selected drugs in patient urine samples and comparable results against reference methods. The method is simple, sensitive and can be considered as an alternative for clinical laboratory analysis of selected drugs.

Simultaneous enantiomeric analysis of non-steroidal anti-inflammatory drugs in environment by chiral LC-MS/MS: A pilot study in Beijing, China

A simple, sensitive and quick method for direct simultaneous chiral analysis of frequently used non-steroidal anti-inflammatory drugs (NSAIDs) (ibuprofen, naproxen and flurbiprofen) in river water by HPLC-MS/MS was established and validated. Chromatographic parameters including the mobile phase composition, pH values, temperature and flow rates were optimized to obtain both satisfactory sensitivity and enantiomeric resolution (Rs≥ 1.0), which suggested the composition and pH values of mobile phase played crucial influence on enantioseparations. The method demonstrated its superiority compared with previous studies regarding to the low MQLs (1.1–37.1 ng/L) and short runtime (< 20 min), enabling quantitative enantiomeric determination of trace level of emerging contaminants in water. The environmental monitoring of receiving water (34 sites along rivers) in Beijing revealed ibuprofen was the most abundant, with mean concentration of 114.9 ng/L and detection frequency of 91%, naproxen was also detectable at all sites from < MQL-43.2 ng/L, both presenting an excess of the S-(+)-enantiomer. Therefore to better understand the ecological risk posed from the trace organic contaminants on the aquatic organisms, chiral pollutants need analyzed at the enantiomeric levels. This is the first to profile the enantiospecific occurrence of NSAIDs in surface water in Beijing, China. It could provide useful information on environmental behaviors of chiral pollutants and facilitate more accurate environmental risk assessment.