Determination of sulfa antibiotic residues in river and particulate matter by field-amplified sample injection-capillary zone electrophoresis

In the present research, field-amplified sample injection–CZE (FASI–CZE) coupled with a diode array detector was established to determine trace level sulfa antibiotic. Sulfathiazole, sulfadiazine, sulfamethazine, sulfadimethoxine, sulfamethoxazole, and sulfisoxazole were selected as analytes for the experiments. The background electrolyte solution consisted of 70.0 mmol/L borax and 60.0 mmol/L boric acid (including 10% methanol, pH 9.1). The plug was 2.5 mmol/L borax, which was injected into the capillary at a pressure of 0.5 psi for 5 s. Then the sample was injected into the capillary at an injection voltage of –10 kV for 20 s. The electrophoretic separation was carried out under a voltage of +19 kV. The capillary temperature was maintained at 20˚C throughout the analysis, and six sulfonamides were completely separated within 35 min. Compared with pressure injection-CZE, the sensitivity of FASI-CZE was increased by 6.25–10.0 times, and the LODs were reduced from 0.2–0.5 to 0.02–0.05 μg/mL. The method was applied to the determination of sulfonamides in river water and particulate matter samples. The recoveries were 78.59–106.59%. The intraday and interday precisions were 2.89–7.35% and 2.77–7.09%, respectively. This provides a simpler and faster method for the analysis of sulfa antibiotic residues in environmental samples.     

Development of a precolumn derivatization HPLC method with diode‐array detection for the determination of amino sugars in peat and soil humic acids

The work is focused on the development of a high‐performance liquid chromatography method with diode‐array detection for the separation and quantitation of the three most abundant amino sugars; d ‐glucosamine, d ‐galactosamine, and d ‐mannosamine. The high‐performance liquid chromatography separation was carried out by reversed‐phase chromatography on Chromolith Performance RP‐18e monolithic column after acid hydrolysis (5 M HCl) and precolumn derivatization of samples using diethyl ethoxymethylenemalonate. Gradient elution and a mobile phase composed of ammonium formate buffer solution (10 mmol/L, pH 3.60) and methanol with flow rate of 1.0 mL/min were used. The monitoring wavelength was set at 280 nm. The limits of detection and quantitation for analytes ranged from 0.017 to 0.122 mg/L and from 0.057 to 0.407 mg/L, respectively. The proposed method was successfully applied for the determination of amino sugars in samples of humic acids isolated from different soils and peat.     

Ultrafast capillary electrophoresis method for the simultaneous determination of ammonium and diphenhydramine in pharmaceutical samples

Ammonium and diphenhydramine are active ingredients commonly found in the same pharmaceutical preparations. We report, for the first time, a sub‐minute method for the simultaneous determination of ammonium and diphenhydramine. The method is based on capillary electrophoresis with capacitively coupled contactless conductivity detection. Both analytes can be quantified in a single run (∼80 injections/h) using 30 mmol/L 2‐(N‐morpholino)ethanesulfonic acid and 15 mmol/L lithium hydroxide (pH 6.0) as background electrolyte. The separation by capillary electrophoresis was achieved on a fused‐silica capillary (50 cm total length, 10 cm effective length, and 50 μm inside diameter). The limits of detection were 0.04 and 0.02 mmol/L for ammonium and diphenhydramine, respectively. The proposed method also provided adequate recovery values for spiked samples (100–106 and 97–104% for ammonium and diphenhydramine, respectively). The results obtained with the new capillary electrophoresis method were compared with those of the high‐performance liquid chromatography method for diphenhydramine and the Kjeldahl method for ammonium and no statistically significant differences were found (95% confidence level).     

Pipette vial dispersive liquid–liquid microextraction combined with high‐performance liquid chromatography for the determination of benzoylurea insecticide in fruit juice

A simple, sensitive, and efficient method of using a pipette vial to perform dispersive liquid–liquid microextraction based on the solidification of floating organic droplets was coupled with high‐performance liquid chromatography (HPLC) and a diode array detector for the preconcentration and analysis of four benzoylurea insecticides in fruit juice. In this method, 1‐dodecanol was used as an extractant, and a snipped pipette was used as an experimental vial to simplify the procedure of collecting and separating solidified extractant. The experimental parameters were optimized using a Plackett–Burman design and one‐factor‐at‐a‐time method. Under the optimal conditions in the water model, the limits of detection for analytes varied from 0.03 to 0.28 μg/L, and the enrichment factors ranged from 147 to 206. Linearity was achieved for diflubenzuron and flufenoxuron in a range of 0.5–500 μg/L, for hexaflumuron in a range of 1–500 μg/L, and for triflumuron in a range of 5–500 μg/L. The correlation coefficients for the analytes ranged from 0.9986 to 0.9994 with recoveries of 91.4–110.9%. Finally, the developed technique was successfully applied to fruit juice samples with acceptable results. The relative standard deviations of the analytes at two spiking levels (50 and 200 μg/L) varied between 0.2 and 4.5%.     

In‐line coupled single drop liquid–liquid–liquid microextraction with capillary electrophoresis for determining fluoroquinolones in water samples

A simple in‐line single drop liquid–liquid–liquid microextraction (SD‐LLLME) coupled with CE for the determination of two fluoroquinolones was developed. The method is capable to quantify trace amount of analytes in water samples and to improve the sensitivity of CE detection. For the SD‐LLLME, a thin layer of organic phase was used to separate a drop of 0.1 M NaOH hanging at the inlet of the capillary from the aqueous donor phase. By this way, the analytes were extracted to the acceptor phase through the organic layer based on their acidic/basic dissociation equilibrium. The drop was immersed into the organic phase during 10 min for extraction and then it is directly injected into the capillary for the analysis. Parameters such as type and volume of organic solvent phase, aqueous donor, and acceptor phases and extraction time and temperature were optimized. The enrichment factor was calculated, resulting 40‐fold for enrofloxacin (ENR) and sixfold for ciprofloxacin (CIP). The linear range were 20–400 μg/L for ENR and 60–400 μg/L for CIP. The detection limits were 10.1 μg/L and 55.3 μg/L for ENR and CIP, respectively, and a good reproducibility was obtained (4.4% for ENR and 5.6% for CIP). Two real water samples were analysed applying the new method and the obtained results presented satisfactory recovery percentages (90–100.3%).     

Field-amplified sample injection combined with pressure-assisted capillary electrophoresis UV detection for the simultaneous analysis of allantoin, uric acid, and malondialdehyde in human plasma

The allantoin/uric acid (All/UA) ratio and malondialdehyde (MDA) plasma levels have been proposed as important markers for monitoring oxidation triggered by the action of free radicals (FR). Here, we describe an easy field amplified sample injection capillary electrophoresis method with UV detection for the separation and quantification of All, UA, and free MDA in human plasma. The plasma samples were simply filtered through centrifugation membrane tubes for protein elimination and directly injected on a capillary without complex cleanup and/or sample derivatization procedures. The use of a run buffer composed of 300 mmol/L sodium borate at pH 10 with 50 mmol/L of N-methyl-d-glucamine and an overimposed pressure/voltage of 0.1 psi during the electrophoretic run allows basline resolution of the analytes within 17 min. The electrokinetic injection allows a detection limit of 15 nmol/L for All, 20 nmol/L for UA and 10 nmol/L for MDA in a plasma sample, thus significantly improving the LOD of previous described methods based on capillary electrophoresis. Precision tests indicate a good repeatability of our method both for migration times (CV = 1.85%) and areas (CV = 2.87%). Moreover, a good reproducibility of intra- and inter-assay tests was obtained (CV = 4.63% and CV = 6.59% respectively). The suitability of the method was tested by measuring analyte levels in 40 healthy volunteers.     

Miniaturized matrix solid‐phase dispersion coupled with supramolecular solvent‐based microextraction for the determination of paraben preservatives in cream samples

An analytical method is presented for the determination of paraben preservatives in semisolid cream samples by matrix solid‐phase dispersion combined with supramolecular solvent‐based microextraction. Due to the oily and sticky nature of the sample matrix, parabens were first extracted from the samples by matrix solid‐phase dispersion using silica as sorbent material with a clean‐up performed with tetrahydrofuran in the elution step. The eluate (500 μL), 1‐decanol (120 μL), and water (4.4 mL) were then mixed in a polyethylene pipette to form supramolecular solvent. Finally, the analytes in the supramolecular solvent were separated and determined by liquid chromatography with ultraviolet detection. Under optimal extraction conditions, the extraction recoveries of the studied compounds were obtained in the range of 63–83%. The limits of detection for the analytes were between 0.03 and 0.04 μg/g. The precision of the method varied between 4.0–6.7 (intraday) and 6.2–7.9% (interday). Finally, the optimized procedure was applied to the determination of the target preservatives in a variety of cream samples (diaper rash, skin allergy, face and hand moisturizing) with satisfactory recoveries (86–102%).     

Core-shell magnetic porous organic polymer for magnetic solid-phase extraction of fluoroquinolone antibiotics in honey samples followed by high-performance liquid chromatography with fluorescence detection

By monomer-mediated in-situ growth synthesis strategy, with hydroquinone and 1,3,5-tris(4-aminophenyl)benzene as monomers, a core-shell magnetic porous organic polymer was synthesized through a simple azo reaction. Based on this, a magnetic solid-phase extraction–high-performance liquid chromatography–fluorescence detection method was proposed for the analysis of fluoroquinolones in a honey sample. With ofloxacin, ciprofloxacin, enrofloxacin, lomefloxacin, and difloxacin as target analytes, factors affecting the extraction efficiency had been optimized. The LODs were 1.5–5.4 ng/L (corresponding to 0.23–0.81 μg/kg in honey). The linear range was 0.005–20 μg/L for difloxacin, 0.01–20 μg/L for ofloxacin, ciprofloxacin and lomefloxacin, and 0.02–20 μg/L for enrofloxacin. The enrichment factor was 84.4–91.7-fold with a high extraction efficiency of 84.4–91.7%. The method was assessed by the analysis of target fluoroquinolones in honey samples, and the recoveries for the spiked samples were 79.3–95.8%. The results indicated that the established magnetic solid-phase extraction–high-performance liquid chromatography–fluorescence detection method is efficient for the analysis of trace fluoroquinolones in honey.     

Rapid determination of antiviral medication ribavirin in different feedstuffs using a novel magnetic molecularly imprinted polymer coupled with high‐performance liquid chromatography

A novel magnetic molecularly imprinted polymer adsorbing material was successfully synthesized to detect ribavirin in animal feedstuff. Molecularly imprinted polymer was prepared through surface polymerization by using ribavirin as template molecule, methyl methacrylate, and γ‐methacryloxypropyl trimethoxy silane functionalized magnetic mesoporous silica as bifunctional monomers, and ethylene diglycidyl ether as crosslinking agent. The prepared magnetic molecularly imprinted polymer was characterized by scanning electron microscopy and infrared spectroscopy. Static and dynamic adsorption experiments and selective adsorption analysis were performed to evaluate the adsorption and selectivity of magnetic molecularly imprinted polymer. Different experiments were conducted to optimize the magnetic solid‐phase extraction conditions. Under optimal experimental conditions, a magnetic molecularly imprinted solid‐phase extraction coupled with high‐performance liquid chromatography method was successfully developed for ribavirin detection. The established method achieved a satisfactory linear range of 0.20–50 mg/L (R² > 0.99) and a low detection limit (0.081 mg/kg). An average recovery of 92–105% with relative standard deviation of <6.5% was obtained upon the application of the developed method to detect ribavirin in real feedstuff samples. Thus, established method can be used for the rapid and simple separation and detection of added ribavirin in feedstuff.     

Magnetic micro‐solid‐phase extraction based on magnetite‐MCM‐41 with gas chromatography–mass spectrometry for the determination of antidepressant drugs in biological fluids

A new facile magnetic micro‐solid‐phase extraction coupled to gas chromatography and mass spectrometry detection was developed for the extraction and determination of selected antidepressant drugs in biological fluids using magnetite‐MCM‐41 as adsorbent. The synthesized sorbent was characterized by several spectroscopic techniques. The maximum extraction efficiency for extraction of 500 μg/L antidepressant drugs from aqueous solution was obtained with 15 mg of magnetite‐MCM‐41 at pH 12. The analyte was desorbed using 100 μL of acetonitrile prior to gas chromatography determination. This method was rapid in which the adsorption procedure was completed in 60 s. Under the optimized conditions using 15 mL of antidepressant drugs sample, the calibration curve showed good linearity in the range of 0.05–500 μg/L (r ² = 0.996–0.999). Good limits of detection (0.008–0.010 μg/L) were obtained for the analytes with good relative standard deviations of <8.0% (n  = 5) for the determination of 0.1, 5.0, and 500.0 μg/L of antidepressant drugs. This method was successfully applied to the determination of amitriptyline and chlorpromazine in plasma and urine samples. The recoveries of spiked plasma and urine samples were in the range of 86.1–115.4%. Results indicate that magnetite micro‐solid‐phase extraction with gas chromatography and mass spectrometry is a convenient, fast, and economical method for the extraction and determination of amitriptyline and chlorpromazine in biological samples.     

Temperature‐controlled liquid–liquid microextraction combined with high‐performance liquid chromatography for the simultaneous determination of diazinon and fenitrothion in water and fruit juice samples

A simple, environmentally benign, and rapid method based on temperature‐controlled liquid–liquid microextraction using a deep eutectic solvent was developed for the simultaneous extraction/preconcentration of diazinon and fenitrothion. The method involved the addition of deep eutectic solvent to the aqueous sample followed by heating the mixture in a 75°C water bath until the solvent was completely dissolved in the aqueous phase. Then, the resultant solution was cooled in an ice bath and a cloudy solution was formed. Afterward, the mixture was centrifuged and the enriched deep eutectic solvent phase was analyzed by high‐performance liquid chromatography with ultraviolet detection for quantification of the analytes. The factors affecting the extraction efficiency were optimized. Under the optimized extraction conditions, the limits of detection for diazinon and fenitrothion were 0.3 and 0.15 μg/L, respectively. The calibration curves for diazinon and fenitrothion exhibited linearity in the concentration range of 1–100 and 0.5–100 μg/L, respectively. The relative standard deviations for five replicate measurements at 10.0 μg/L level of analytes were less than 2.8 and 4.5% for intra‐ and interday assays, respectively. The developed method was successfully applied to the determination of diazinon and fenitrothion in water and fruit juice samples.     

Determination of ultraviolet filter compounds in environmental water samples using membrane‐protected micro‐solid‐phase extraction

A method based on membrane‐protected micro‐solid‐phase extraction coupled with gas chromatography and mass spectrometry was developed for the determination of six ultraviolet filter compounds in various aqueous media. Multiwalled carbon nanotubes as the sorbent were encapsulated in a sealed polypropylene membrane packet and immersed in the sample to extract the analytes, and then dichloromethane was used for desorption purpose. The method was sensitive enough for quantitative analysis of the target analytes, with limits of quantification between 0.01 and 0.06 μg/L, and produced a linear response (R² > 0.991) over the calibration range (0.05–6 μg/L). The obtained reproducibility was practically suitable with relative standard deviation values of less than 14% in pure water (spiked at 0.20/μg L) and less than 15% in real samples. The optimized method was applied for the analysis of real water samples with varying matrix complexity: tap, river, and dam water; geothermal spa; and sewage treatment plant effluent. Various levels and patterns of contamination were observed in the examined samples, while the sample from spa was the most contaminated, regarding the target analytes. Matrix spikes and matrix spike replicates were also analyzed to validate the technique for analysis of real aqueous samples, and satisfactory results were achieved.     

Application of sunflower stalk‐carbon nitride nanosheets as a green sorbent in the solid‐phase extraction of polycyclic aromatic hydrocarbons followed by high‐performance liquid chromatography

A green biocomposite of sunflower stalks and graphitic carbon nitride nanosheets has been applied as a solid‐phase extraction adsorbent for sample preparation of five polycyclic aromatic hydrocarbons in different solutions using high‐performance liquid chromatography with ultraviolet detection. Before the modification, sunflower stalks exhibited relatively low adsorption to the polycyclic aromatic hydrocarbons extraction. The modified sunflower stalks showed increased adsorption to the analytes extraction due to the increase in surface and existence of a π–π interaction between the analytes and graphitic carbon nitride nanosheets on the surface. Under the optimal conditions, the limits of detection and quantification for five polycyclic aromatic hydrocarbons compounds could reach 0.4–32 and 1.2–95 ng/L, respectively. The method accuracy was evaluated using recovery measurements in spiked real samples and good recoveries from 71 to 115% with relative standard deviations of <10% have been achieved. The developed method was successfully applied for polycyclic aromatic hydrocarbons determination in various samples—well water, tap water, soil, vegetable, and barbequed meat (kebab)—with analytes contents ranging from 0.065 to 13.3 μg/L. The prepared green composite as a new sorbent has some advantages including ease of preparation, low cost, and good reusability.     

Simultaneous determination of 4‐hydroxyphenyl lactic acid, 4‐hydroxyphenyl acetic acid,and 3,4‐hydroxyphenyl propionic acid in human urine by ultra‐high performance liquid chromatography with fluorescence detection

A simple and reliable method was established for simultaneous determination of 4‐hydroxyphenyl acetic acid, 4‐hydroxyphenyl lactic acid, and 3,4‐hydroxyphenyl propionic acid in human urine by high‐performance liquid chromatography with fluorescence detection. Solid‐phase extraction was used to eliminate the interferences in urine. The separation of three analytes was achieved using a C₁₈ column and a mobile phase formed by a 95:5 v/v mixture of 50 mmol/L ammonium acetate buffer at pH 6.8 that contained 5 mmol/L tetrabutyl ammonium bromide and acetonitrile. Under the optimized conditions, the detection limits of 4‐hydroxyphenyl acetic acid, 4‐hydroxyphenyl lactic acid, and 3,4‐hydroxyphenyl propionic acid were 4.8 × 10⁻³, 8.80 × 10⁻³, and 9.00 × 10⁻³ mg/L, respectively, and the recoveries were in the range of 85.0–120.0% with relative standard deviations of 1.5–3.1%. This method was used to analyze urine samples from breast cancer patients, healthy people and post‐surgery breast cancer patients. Significant differences in urinary levels of 4‐hydroxyphenyl acetic acid and 4‐hydroxyphenyl lactic acid could be found between the breast cancer patients group and other two groups. No effect of age and sex was observed on the urinary levels of 4‐hydroxyphenyl acetic acid and 4‐hydroxyphenyl lactic acid. This method might be helpful for cancer biomarkers discovery in urine.     

On-line determination of aliphatic amines in water using in-tube solid-phase microextraction-assisted derivatisation in in-valve mode for processing large sample volumes in LC

This paper describes a cost-effective procedure for the analysis of short-chain aliphatic amines in water samples using a solid-phase microextraction device. Analyte preconcentration and derivatisation were effected into a capillary column coated with 95% polydimethylsiloxane–5% polydiphenylsiloxane, which was used as the injection loop of a Rheodyne injection valve. The coating was previously loaded with the derivatisation reagent, 9-fluorenylmethyl chloroformate. A volume of 1 mL of samples was then drawn into the capillary column, and the extracted analytes were left to react on the capillary coating for 5 min. Next, the capillary column was cleaned by passing water. Finally, the injection valve was rotated, and the derivatives formed were dynamically desorbed and transferred to the analytical column into the mobile phase. Methylamine, ethylamine, propylamine, n-butylamine and n-pentylamine were selected as model compounds. Excellent sensitivity was achieved, being the limits of detection of 15–200 μg/L when using UV detection and of 0.1–0.4 μg/L by fluorescence.     

Determination of 11 priority pollutant phenols in wastewater using dispersive liquid—liquid microextraction followed by high-performance liquid chromatography—diode-array detection

Dispersive liquid—liquid microextraction coupled with high-performance liquid chromatography—diode-array detection was applied for the extraction and determination of 11 priority pollutant phenols in wastewater samples. The analytes were extracted from a 5-mL sample solution using a mixture of carbon disulfide as the extraction solvent and acetone as the dispersive solvent. After extraction, solvent exchange was carried out by evaporating the solvent and then reconstituting the residue in a mixture of methanol–water (30:70). The influences of different experimental dispersive liquid—liquid microextraction parameters such as extraction solvent type, dispersive solvent type, extraction and dispersive solvent volume, salt addition, and pH were studied. Under optimal conditions, namely pH 2, 165-μL extraction solvent volume, 2.50-mL dispersive solvent volume, and no salt addition, enrichment factors and limits of detection ranged over 30–373 and 0.01–1.3 μg/L, respectively. The relative standard deviation for spiked wastewater samples at 10 μg/L of each phenol ranged between 4.3 and 19.3% (n = 5). The relative recovery for wastewater samples at a spiked level of 10 μg/L varied from 65.5 to 108.3%.     

Carbon nanospheres as solid‐phase microextraction coating for the extraction of polycyclic aromatic hydrocarbons from water and soil samples

A solid‐phase microextraction with carbon nanospheres coated fiber coupled with gas chromatographic detection was established for the determination of eight polycyclic aromatic hydrocarbons (naphthalene, biphenyl, acenaphthene, fluorine, phenanthrene, anthracene, fluoranthene, and pyrene) in water and soil samples. The experimental parameters (extraction temperature, extraction time, stirring rate, headspace volume, salt content, and desorption temperature) which affect the extraction efficiency were studied. Under the optimized conditions, good linearity between the peak areas and the concentrations of the analytes was achieved in the concentration range of 0.5‐300 ng/mL for water samples, and in the concentration range of 6.0‐2700 ng/g for soil samples. The detection limits for the analytes were in the range of 0.12‐0.45 ng/mL for water samples, and in the range of 1.53‐2.70 ng/g for soil samples. The method recoveries of the polycyclic aromatic hydrocarbons for spiked water samples were 80.10‐120.1% with relative standard deviations less than 13.9%. The method recoveries of the analytes for spiked soil samples were 80.40‐119.6% with relative standard deviations less than 14.4%. The fiber was reused over 100 times without a significant loss of extraction efficiency.     

Preparation of a magnetic porous carbon with hierarchical structures from waste biomass for the extraction of some carbamates

In this study, corn stalk was used to synthesize a magnetic adsorbent by pyrolysis together with KHCO₃ as the chemical activator and iron(III) salt as the magnetic reagent. The characterization by scanning electron microscopy, transmission electron microscopy and N₂ adsorption–desorption analysis showed that the magnetic carbon adsorbent had a structure of hierarchical pores with a high specific surface area. To evaluate its adsorption performance, the adsorbent was used for the extraction of carbamates pesticides (propoxur, isoprocarb and fenobucarb) from water and zucchini samples before high‐performance liquid chromatography analysis. The result showed that the adsorbent had a good adsorption capability for the analytes. Under the optimized conditions, a good linearity for the analytes existed in the range of 0.1–100.0 ng/mL for water samples and 0.5–100.0 ng/g for zucchini samples with the correlation coefficients of 0.9992–0.9998. The limits of detection for the analytes at a signal to noise ratio of 3 were 0.03 ng/mL for water samples and 0.20–0.50 ng/g for zucchini samples.     

Quality by design-based capillary electrophoresis method development for the quantitative analysis of four iridoid compounds in Gentiana macrophylla Radix

In this study, the capillary electrophoresis-photodiode array detector was employed for the analysis of four iridoid compounds in Gentiana macrophylla Radix (RGM), and the method was optimized based on the concept of analytical quality by design (AQbD). The peak areas relative standard deviation (n = 3) and resolution of the four analytes were selected as critical method attributes. Fractional factorial design test combined with Pareto analysis were employed to screen critical method parameters (buffer concentration, pH, sodium dodecyl sulfate [SDS] micelle concentration, temperature, and voltage). Subsequently, three main factors (buffer concentration, buffer pH, and SDS concentration) were selected by central composite design test for constructing the design space. The optimal separation conditions as follows: capillary column (50.2 cm × 50 µm, detection length 40 cm). Working background electrolyte consisted of 51 mmol/L borax solution (pH = 9.47) and 40 mmol/L SDS. The samples were injected by pressure (5 s at 0.5 psi) and the detection was performed at 254 nm. Applied voltage was 20 kV and column temperature was 23°C. The developed method is rapid and reliable for the quantitative analysis of four iridoid compounds in RGM, providing a reference for the application of AQbD concept in the analysis of natural products.     

Application of a novel nylon needle filter-based solid-phase extraction device to determination of 1-hydroxypyrene in urine

In this work, a simple and miniaturized solid-phase extraction device was constructed by connecting a commercial nylon needle filter to a syringe, which was applied for extracting 1-hydroxypyrene from a urine sample via hydrophobic and hydrogen bond interactions. The nylon membrane in the needle filter acted as the solid-phase extraction adsorbent, meanwhile, it filtered the particles in the urine sample. To obtain high extraction efficiency, key parameters influencing extraction recovery were investigated. The entire pretreatment process was accomplished within 5 min under the optimal conditions. By coupling high-performance liquid chromatography–ultraviolet, a rapid, low-cost, and convenient nylon needle filter-based method was established for the analysis of 1-hydroxypyrene in a complex urine matrix. Within the linearity range of 0.2–1000 μg/L, the method exhibited a satisfactory correlation coefficient (R = 0.9999). The limit of detection was 0.06 μg/L, and the recoveries from urine sample spiked with three concentrations (5, 20, and 100 μg/L) ranged from 105.8% to 113.1% with the relative standard deviations less than 6.7% (intra-day, n = 6) and 8.9% (inter-day, n = 4). Finally, the proposed method was successfully applied for detecting 1-hydroxypyrene in urine samples from college students, smokers, gas station workers, and chip factory workers. The detected concentration in actual urine samples ranged from 0.46 to 5.26 μg/L. Taken together, this simple and cost-effective nylon needle filter-based solid-phase extraction device showed an excellent application potential for pretreating hydrophobic analytes from aqueous samples.