Solvent‐vapor‐assisted liquid–liquid microextraction: A novel method for the determination of phthalate esters in aqueous samples using GC–MS

A novel liquid–liquid microextraction method, namely, solvent‐vapor‐assisted liquid–liquid microextraction for the determination of dimethyl phthalate, diethyl phthalate, dibutyl phthalate and bis(2‐ethylhexyl) phthalate in the aqueous samples using gas chromatography with mass spectrometry was developed. In the proposed method, extracting solvent was heated, and solvent vapor as the extracting phase was injected into the sample solution. As a result of the low temperature of the sample solution and higher density of the extracting phase than the aqueous medium, solvent vapor was condensed and an organic‐phase drop formed in the bottom of sample tube. Because of the gas status of the extracting solvent, the surface area between the extracting solvent and the aqueous sample was remarkably high. Under the optimized conditions, tetrachloride carbon was used as an extracting solvent. The method shows high coefficient of determination (R ²) values in the range of 0.5–200 and 1.0–200 ng/mL for the target analytes. Enrichment factors and limits of detection for the studied phthalates are obtained in the ranges of 2800–3000 and 0.15–0.3 ng/mL, respectively. Recoveries and relative standard deviations were in the range of 80.0–100.0 and 2.2–7.8%, respectively. The proposed method successfully used for analysis of several aqueous samples.     

Determination of phthalic acid esters in Chinese white spirit using dispersive liquid–liquid microextraction coupled with sweeping β‐cyclodextrin‐modified micellar electrokinetic chromatography

A simple method that consumes low organic solvent is proposed for the analysis of phthalic acid esters in Chinese white spirit using dispersive liquid–liquid microextraction coupled with sweeping‐micellar electrokinetic chromatography. Tetrachloromethane and white‐spirit‐containing ethanol were used as the extraction and dispersing solvents, respectively. The electrophoresis separation buffer was composed of 5 mM β‐cyclodextrin, 50 mM sodium dodecyl sulfate and 25 mM borate buffer (pH 9.2) with 9% acetonitrile, enabling the baseline resolution of the analytes within 13 min. Under the optimum conditions, satisfactory linearities (5–1000 ng/mL, r ≥ 0.9909), good reproducibility (RSD ≤ 6.7% for peak area, and RSD ≤ 2.8% for migration time), low detection limits (0.4–0.8 ng/mL) and acceptable recovery rates (89.6–105.7%) were obtained. The proposed method was successfully applied to 22 Chinese white spirits, and the content of dibutyl phthalate in 55% of the samples exceeded the Specific Migration Limit of 0.3 mg/kg established by the domestic and international regulations.     

Magnetic solid‐phase extraction or dispersive liquid–liquid microextraction for pyrethroid determination in environmental samples

The determination of 15 pyrethroids in soil and water samples was carried out by gas chromatography with mass spectrometry. Compounds were extracted from the soil samples (4 g) using solid–liquid extraction and then salting‐out assisted liquid–liquid extraction. The acetonitrile phase obtained (0.8 mL) was used as a dispersant solvent, to which 75 μL of chloroform was added as an extractant solvent, submitting the mixture to dispersive liquid–liquid microextraction. For the analysis of water samples (40 mL), magnetic solid‐phase extraction was performed using nanocomposites of magnetic nanoparticles and multiwalled carbon nanotubes as sorbent material (10 mg). The mixture was shaken for 45 min at room temperature before separation with a magnet and desorption with 3 mL of acetone using ultrasounds for 5 min. The solvent was evaporated and reconstituted with 100 μL acetonitrile before injection. Matrix‐matched calibration is recommended for quantification of soil samples, while water samples can be quantified by standards calibration. The limits of detection were in the range of 0.03–0.5 ng/g (soil) and 0.09–0.24 ng/mL (water), depending on the analyte. The analyzed environmental samples did not contain the studied pyrethroids, at least above the corresponding limits of detection.     

Phytic acid induced three‐dimensional graphene for the enrichment of phthalate esters from bottled water and sports beverage samples

A three‐dimensional graphene was synthesized through a hydrothermal reaction of graphene oxide with phytic acid. The microstructure and morphology of the phytic acid induced three‐dimensional graphene were investigated by nitrogen adsorption–desorption isotherms, scanning electron microscopy, and transmission electron microscopy. With a large surface area and three‐dimensional structure, the graphene was used as the solid‐phase extraction adsorbent for the extraction of phthalate esters from bottled water and sports beverage samples before high‐performance liquid chromatographic analysis. The results indicated that the graphene was efficient for the solid‐phase extraction of phthalate esters. The limits of detection (S/N = 3) of the method for the analytes were 0.02–0.03 ng/mL for the water samples and 0.03–0.15 ng/mL for the sports beverage sample. The limits of quantitation (S/N = 9) for the analytes were 0.06–0.09 ng/mL for water samples and 0.09–0.45 ng/mL for sports beverage sample. The calibration curves for the phthalate esters by the method had a good linearity from 0.1 to 80.0 ng/mL with correlation coefficients larger than 0.9997. The recoveries of the analytes for the method fell in the range of 86.7–116.2% with the relative standard deviations between 1.5 and 6.8%.     

New application of chitosan‐grafted polyaniline in dispersive solid‐phase extraction for the separation and determination of phthalate esters in milk using high‐performance liquid chromatography

Chitosan‐grafted polyaniline was synthesized and applied as a sorbent for the preconcentration of phthalate esters in dispersive solid‐phase extraction. By coupling dispersive solid‐phase extraction with high‐performance liquid chromatography and response surface methodology (central composite design), a reliable, sensitive, and cost‐effective method for simultaneous determination of phthalate esters including dimethyl phthalate, di‐n‐butyl phthalate, and di(2‐ethylhexyl)phthalate was developed. The morphology of sorbent had been studied by scanning electron microscopy and its chemical structure confirmed by Fourier transform infrared spectroscopy. Under optimum condition, good linearity was observed in the range of 5.0–5000.0 ng/mL. The limits of detection (S/N = 3) and limits of quantification (S/N = 10) were 0.1–0.3 and 0.3–1 ng/mL, respectively. The relative standard deviations were less than 8.8%. Finally, this procedure was employed for extraction of trace amounts of phthalic acid esters in milk samples, the relative recoveries ranged from 82 to 103%.     

Determination of phthalates in beverages using multiwalled carbon nanotubes dispersive solid‐phase extraction before HPLC–MS

A microdispersive solid‐phase extraction method has been developed using multiwalled carbon nanotubes of 110–170 nm diameter and 5–9 μm length for the extraction of a group of nine phthalic acid esters (i.e., bis(2‐methoxyethyl) phthalate, bis‐2‐ethoxyethyl phthalate, dipropyl phthalate, butylbenzyl phthalate, bis‐2‐n‐butoxyethyl phthalate, bis‐isopentyl phthalate, bis‐n‐pentyl phthalate, dicyclohexyl phthalate, and di‐n‐octyl phthalate) from tap water as well as from different beverages commercialized in plastic bottles (mineral water, lemon‐ and apple‐flavored mineral water, and an isotonic drink). Determination was carried out by high‐performance liquid chromatography coupled to mass spectrometry. The extraction procedure was optimized following a step‐by‐step approach, being the optimum extraction conditions: 50 mL of each sample at pH 6.0, 80 mg of sorbent, and 25 mL of acetonitrile as elution solvent. To validate the methodology, matrix‐matched calibration and a recovery study were developed, obtaining determination coefficients >0.9906 and absolute recovery values between 70 and 117% (with relative standard deviations < 17%) in all cases. The limits of quantification of the method were between 0.173 and 1.45 μg/L. After the evaluation of the matrix effects, real samples were also analyzed, finding butylbenzyl phthalate in all samples (except in apple‐flavored mineral water), though at concentrations below its limit of quantification of the method.     

Comparison of air‐agitated liquid–liquid microextraction and ultrasound‐assisted emulsification microextraction for polycyclic aromatic hydrocarbons determination in hookah water

In this work, two disperser‐free microextraction methods, namely, air‐agitated liquid–liquid microextraction and ultrasound‐assisted emulsification microextraction are compared for the determination of a number of polycyclic aromatic hydrocarbons in aqueous samples, followed by gas chromatography with flame ionization detection. The effects of various experimental parameters upon the extraction efficiencies of both methods are investigated. Under the optimal conditions, the enrichment factors and limits of detection were found to be in the ranges of 327–773 and 0.015–0.05 ng/mL for air‐agitated liquid–liquid microextraction and 406–670 and 0.015–0.05 ng/mL for ultrasound‐assisted emulsification microextraction, respectively. The linear dynamic ranges and extraction recoveries were obtained to be in the range of 0.05–120 ng/mL (R² ≥ 0.995) and 33–77% for air‐agitated liquid–liquid microextraction and 0.05–110 ng/mL (R² ≥ 0.994) and 41–67% for ultrasound‐assisted emulsification microextraction, respectively. To investigate this common view among some people that smoking hookah is healthy due to the passage of smoke through the hookah water, samples of both the hookah water and hookah smoke were analyzed.     

Desirability function approach for the optimization of an in‐syringe ultrasound‐assisted emulsification‐microextraction method for the simultaneous determination of amlodipine and nifedipine in plasma samples

In the present study, an in‐syringe ultrasound‐assisted emulsification‐microextraction using a low‐density organic solvent was developed for simultaneous extraction and pre‐concentration of amlodipine besylate and nifedipine from plasma samples. The extracts were analyzed by high‐performance liquid chromatography with UV detection. Central composite design combined with desirability function was applied to find out the optimal experimental conditions providing the highest global extraction efficiency. The optimal conditions identified were volume of the extracting solvent 45 μL, ionic strength 18.95% w/v, sonication time 2.58 min, and centrifugation time 3 min. Under the optimal conditions, the proposed method was evaluated, and applied to the analysis of amlodipine besylate and nifedipine in plasma samples. The validation results of the method indicated a wide linear range (2–1200 ng/mL) with a good linearity (r² >0.9991) and low detection limits (0.17 ng/mL for amlodipine besylate and 0.15 ng/mL for nifedipine) with RSD less than 5.2% for both components, both in intra‐ and inter‐day precision studies. The applicability of the proposed in‐syringe ultrasound‐assisted emulsification‐microextraction coupled to high‐performance liquid chromatography with UV detection method was demonstrated by analyzing the drugs in spiked plasma samples.     

Optimization of multiwalled carbon nanotubes reinforced hollow‐fiber solid–liquid‐phase microextraction for the determination of polycyclic aromatic hydrocarbons in environmental water samples using experimental design

A novel design of hollow‐fiber liquid‐phase microextraction containing multiwalled carbon nanotubes as a solid sorbent, which is immobilized in the pore and lumen of hollow fiber by the sol–gel technique, was developed for the pre‐concentration and determination of polycyclic aromatic hydrocarbons in environmental water samples. The proposed method utilized both solid‐ and liquid‐phase microextraction media. Parameters that affect the extraction of polycyclic aromatic hydrocarbons were optimized in two successive steps as follows. Firstly, a methodology based on a quarter factorial design was used to choose the significant variables. Then, these significant factors were optimized utilizing central composite design. Under the optimized condition (extraction time = 25 min, amount of multiwalled carbon nanotubes = 78 mg, sample volume = 8 mL, and desorption time = 5 min), the calibration curves showed high linearity (R ² = 0.99) in the range of 0.01–500 ng/mL and the limits of detection were in the range of 0.007–1.47 ng/mL. The obtained extraction recoveries for 10 ng/mL of polycyclic aromatic hydrocarbons standard solution were in the range of 85–92%. Replicating the experiment under these conditions five times gave relative standard deviations lower than 6%. Finally, the method was successfully applied for pre‐concentration and determination of polycyclic aromatic hydrocarbons in environmental water samples.     

Simple and rapid determination of phthalates using microextraction by packed sorbent and gas chromatography with mass spectrometry quantification in cold drink and cosmetic samples

A simple and rapid method using microextraction by packed sorbent coupled with gas chromatography and mass spectrometry has been developed for the analysis of five phthalates, namely, diethyl phthalate, benzyl‐n‐butyl phthalate, dicyclohexyl phthalate, di‐n‐butyl phthalate, and di‐n‐propyl phthalate, in cold drink and cosmetic samples. The various parameters that influence the microextraction by packed sorbent performance such as extraction cycle (extract–discard), type and amount of solvent, washing solvent, and pH have been studied. The optimal conditions of microextraction using C₁₈ as the packed sorbent were 15 extraction cycles with water as washing solvent and 3 × 10 μL of ethyl acetate as the eluting solvent. Chromatographic separation was also optimized for injection temperature, flow rate, ion source, interface temperature, column temperature gradient and mass spectrometry was evaluated using the scan and selected ion monitoring data acquisition mode. Satisfactory results were obtained in terms of linearity with R² >0.9992 within the established concentration range. The limit of detection was 0.003–0.015 ng/mL, and the limit of quantification was 0.009–0.049 ng/mL. The recoveries were in the range of 92.35–98.90% for cold drink, 88.23–169.20% for perfume, and 88.90–184.40% for cream. Analysis by microextraction by packed sorbent promises to be a rapid method for the determination of these phthalates in cold drink and cosmetic samples, reducing the amount of sample, solvent, time and cost.     

Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid‐phase extraction combined with ultrasound‐assisted dispersive liquid–liquid microextraction and UHPLC–MS/MS

A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid‐phase extraction combined with ultrasound‐assisted dispersive liquid–liquid microextraction before ultra‐high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid‐phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid–liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0–400 (tebuconazole, diniconazole, and hexaconazole) and 4.0–800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5–1.1 and 1.8–4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained.     

Preconcentration and determination of 2‐mercaptobenzimidazole by dispersive liquid–liquid microextraction and experimental design

A method was developed to determine 2‐mercaptobenzimidazole in water and urine samples using dispersive liquid–liquid microextraction technique coupled with ultraviolet–visible spectrophotometry. It was essential to peruse the effect of all parameters that can likely influence the performance of extraction. The influence of parameters, such as dispersive and extraction solvent volume and sample volume, on dispersive liquid–liquid microextraction was studied. The optimization was carried out by the central composite design method. The central composite design optimization method resulted in 1.10 mL dispersive solvent, 138.46 μL extraction solvent, and 4.46 mL sample volume. Under the optimal terms, the calibration curve was linear over the range of 0.003–0.18 and 0.007–0.18 μg/mL in water and urine samples, respectively. The limit of detection and quantification of the proposed approach for 2‐mercaptobenzimidazole were 0.013 and 0.044 μg/mL in water samples and 0.016 and 0.052 μg/mL in urine samples, respectively. The method was successfully applied to determination of 2‐mercaptobenzimidazole in urine and water samples.     

Magnetic N‐doped mesoporous carbon as an adsorbent for the magnetic solid‐phase extraction of phthalate esters from soft drinks

A new kind of magnetic N‐doped mesoporous carbon was prepared by the one‐step carbonization of a hybrid precursor (glucose, melamine, and iron chloride) in a N₂ atmosphere with a eutectic salt (KCl/ZnCl₂) as the porogen. The obtained magnetic N‐doped mesoporous carbon showed excellent characteristics, such as strong magnetic response, high surface area, large pore volume, and abundant π‐electron system, which endow it with a great potential as a magnetic solid‐phase extraction adsorbent. To evaluate its adsorption performance, the magnetic N‐doped mesoporous carbon was used for the extraction of three phthalate esters from soft drink samples followed by high‐performance liquid chromatographic analysis. Under the optimum conditions, the developed method showed a good linearity (1.0–120.0 ng/mL), low limit of detection (0.1–0.3 ng/mL, S/N = 3), and good recoveries (83.2–119.0%) in soft drink samples. The results indicated that the magnetic N‐doped mesoporous carbon has an excellent adsorption capacity for phthalate esters and the present method is simple, accurate, and highly efficient for the extraction and determination of phthalate esters in complex matrix samples.     

Ultrasound‐assisted supramolecular‐solvent‐based microextraction combined with high‐performance liquid chromatography for the analysis of chlorophenols in environmental water samples

An efficient, inexpensive and environmentally benign ultrasound‐assisted supramolecular‐solvent‐based microextraction technique combined with high‐performance liquid chromatography was used for the determination of chlorophenols in environmental water samples. Different factors such as amount of decanoic acid, volume of tetrahydrofuran, pH of the sample, ultrasound time and ionic strength were investigated and optimized. The optimized extraction conditions were 60 mg decanoic acid, 1.5 mL tetrahydrofuran, 3 min ultrasound time, without salt addition. Under this condition, the extraction recoveries were 83.0–89.3 with preconcentration factors of 94–102. The calibration curves were linear from 5.0–400.0 ng/mL with square of the correlation coefficient higher than 0.9998 and the limits of detection were between 1.5–2.0 ng/mL. The values of intra‐ and inter‐day relative standard deviations were 3.2–6.0 and 7.3–8.0%, respectively. Analysis of different samples showed that the concentration of 2,5‐dichlorophenol in Babolrood river water was 80.6 ng/mL.     

Separation and pre‐concentration of glucocorticoids in water samples by ionic liquid supported vortex‐assisted synergic microextraction and HPLC determination

We have developed a synergic microextraction procedure based on ionic liquid for the pre‐concentration and determination of glucocorticoids in water samples. Using nonionic surfactant Triton X‐100 (TX‐100) as synergic reagent, 1‐butyl‐3‐methylimidazolium hexa‐fluorophosphate accomplished extraction rapidly without heating in water bath. One key property of ionic liquids that highlights their potential is their wide liquid temperature range. The improved extraction was named as ionic liquid supported vortex‐assisted synergic microextraction. Compared with the traditional liquid–liquid extraction and cloud point extraction, ionic liquid supported vortex‐assisted synergic microextraction was accomplished in 8 min with considerably high recovery. The proposed method greatly improved the sensitivity of HPLC for the determination of glucocorticoids. The results obtained indicated a good linearity with the correlation coefficient of 0.997 over the range of 0.6–300 ng/mL and high sensitivity with LODs of 4.11, 9.19, and 7.50 ng/mL for hydrocortisone butyrate, beclomethasone dipropionate, and nandrolone phenylpropionate, respectively. The RSD of the method was 1.57–1.81% (n = 6) with enrichment factor of 99.85, and good recovery (≥97.24%). The method was successfully applied to the determination of glucocorticoids in mineral water, water of Dianchi lake, and tap water samples.     

Polymer phase transition characteristics coupled with GC‐MS for the determination of phthalate esters

Phthalate esters are easily released from plastics materials and migrate into the soil and water environment, causing serious pollution and posing a great threat to the health of human beings. A novel temperature‐sensitive extractant combined with liquid–liquid microextraction was developed to preconcentrate three phthalates in the water environment. To optimize the extraction efficiency for the three phthalate esters, various parameters, including polymer molecular weight, salt type, salt addition, adsorption time, desorption solvent, desorption volume, and desorption time have been studied. Under optimal conditions, limits of detection and limits of quantification were in the range of 0.007–0.120 and 0.021–0.350 µg/L, respectively. Linearities varied in the range of 5–1000 µg/L, with the correlation coefficients of 0.9867–0.9997. The preconcentration factors were in the range of 25–75. The relative recoveries of the three phthalate esters were in the range of 82.2–105.6% at the spiked levels. The relative standard deviations were in the range of 0.7–9.2% based on triplicate measurements. The results indicate that the temperature‐sensitive material is a good extractant for phthalate esters in water samples.     

Determination of atenolol in human plasma using ionic‐liquid‐based ultrasound‐assisted in situ solvent formation microextraction followed by high‐performance liquid chromatography

An efficient analytical method called ionic‐liquid‐based ultrasound‐assisted in situ solvent formation microextraction followed by high‐performance liquid chromatography was developed for the determination of atenolol in human plasma. A hydrophobic ionic liquid (1‐butyl‐3‐methylimidazolium hexafluorophosphate) was formed by the addition of a hydrophilic ionic liquid (1‐butyl‐3‐methylimidazolium tetrafluoroborate) to a sample solution containing an ion‐pairing agent during microextraction. The analyte was extracted into the ionic liquid phase while the microextraction solvent was dispersed throughout the sample by utilizing ultrasound. The sample was then centrifuged, and the extracting phase retracted into the microsyringe and injected to liquid chromatography. After optimization, the calibration curve showed linearity in the range of 2–750 ng/mL with the regression coefficient corresponding to 0.998. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.5 and 2 ng/mL, respectively. A reasonable relative recovery range of 90–96.7% and satisfactory intra‐assay (4.8–5.1%, n = 6) and interassay (5.0–5.6%, n = 9) precision along with a substantial sample clean‐up demonstrated good performance of the procedure. It was applied for the determination of atenolol in human plasma after oral administration and some pharmacokinetic data were obtained.     

Ultrasound‐assisted dispersive liquid–liquid microextraction combined with gas chromatography‐mass spectrometry in negative chemical ionization mode for the determination of polybrominated diphenyl ethers in water

A simple and economical method for the determination of eight polybrominated diphenyl ethers (BDE‐28, 47, 99, 100,153,154,183, and 209) in water was developed. This method involves the use of ultrasound‐assisted dispersive liquid–liquid microextraction combined with GC‐MS in negative chemical ionization mode. Various parameters affecting the extraction efficiency, including the type and volume of extraction and dispersive solvents, salt concentration, extraction time, and ultrasonic time, were investigated. A volume of 1.0 mL of acetone (dispersive solvent) containing 10 μL tetrachloroethylene (extraction solvent) was injected into 5.0 mL of water samples and then emulsified by ultrasound for 2.0 min to produce the cloudy solution. Under the optimal condition, the enrichment factors for the eight PBDEs were varied from 845‐ to 1050‐folds. Good linearity was observed in the range of 1.0–200 ng L^?1 for BDE‐28, 47, 99, and 100; 5.0–200 ng L^?1 for BDE‐153, 154, and 183; and 5.0–500 ng L^?1 for BDE‐209. The RSD values were in the range of 2.5–8.4% (n = 5) and the LODs ranged from 0.40 to 2.15 ng L^?1 (S/N = 3). The developed method was applied for the determination of eight BPDEs in the river and lake water samples, and the mean recoveries at spiking levels of 5.0 and 50.0 ng L^?1 were in the range of 70.6–105.1%.     

Up‐and‐down shaker‐assisted ionic liquid‐based dispersive liquid—liquid microextraction of benzophenone‐type ultraviolet filters

Sun protection is an important part of our lives. UV filters are widely used to absorb solar radiation in sunscreens. However, excess UV filters constitute persistent groups of organic micropollutants present in the environment. An environmentally friendly ionic‐liquid‐based up‐and‐down shaker‐assisted dispersive liquid?liquid microextraction device combined with ultra‐performance liquid chromatography coupled with photodiode‐array detection has been developed to preconcentrate three UV filters (benzophenone, 2‐hydroxy‐4‐methoxybenzophenone, 2,2′‐dihydroxy‐4‐methoxybenzophenone) from field water samples. In this method, the optimal conditions for the proposed extraction method were: 40 μL [C₈MIM][PF₆] as extraction solvent and 200 μL methanol as disperser solvent were used to extract the UV filters. After up‐and‐down shaking for 3 min, the aqueous solution was centrifuged at 5000 rpm speed, then using microtube to collect the settled extraction solvent and using ultra‐performance liquid chromatography for further analysis. Quantification results indicated that the linear range was 2–1000 ng/mL. The LOD of this method was in the range 0.2–1.3 ng/mL with r² ≥ 0.9993. The relative recovery in studies of different types of field water samples was in the range 92–120%, and the RSD was 2.3–7.1%. The proposed method was also applied to the analysis of field samples.     

Polyethylene glycol grafted flower‐like cupric nano oxide for the hollow‐fiber solid‐phase microextraction of hexaconazole,penconazole, and diniconazole in vegetable samples

A simple, rapid, highly efficient, and reliable sample preparation method has been developed for the extraction and analysis of triazole pesticides from cucumber, lettuce, bell pepper, cabbage, and tomato samples. This new sorbent in the hollow‐fiber solid‐phase microextraction method is based on the synthesis of polyethylene glycol‐polyethylene glycol grafted flower‐like cupric oxide nanoparticles using sol–gel technology. Afterward, the analytes were analyzed by high‐performance liquid chromatography with ultraviolet detection. The main parameters that affect microextraction efficiency were evaluated and optimized. This method has afforded good linearity ranges (0.5–50 000 ng/mL for hexaconazol, 0.012–50 000 ng/mL for penconazol, and 0.02–50 000 ng/mL for diniconazol), adequate precision (2.9–6.17%, n = 3), batch‐to‐batch reproducibility (4.33–8.12%), and low instrumental LODs between 0.003 and 0.097 ng/mL (n = 8). Recoveries and enrichment factors were 85.46–97.47 and 751–1312%, respectively.