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1.
Xiaojia Huang Ningning QiuDongxing Yuan Qingmei Lin 《Journal of chromatography. A》2010,1217(16):2667-2673
In this study, a novel mixed mode monolithic material was prepared and acted as the SBSE coating. The monolithic material was prepared by in situ copolymerization of methacrylic acid-3-sulfopropyl ester potassium salt (MASE) and divinylbenzene (DB) in the presence of a porogen solvent containing cyclohexanol, 1-dodecanol, and water with azobisisobutyronitrile as initiator. The influences of the contents of the porogen solvent and monomer in the polymerization mixture on the extraction performance were investigated thoroughly. Several characteristic techniques, such as elemental analysis, scanning electron microscopy and infrared spectroscopy were used to characterize the monolithic material. To achieve optimum extraction performance for quinolones, several parameters, including pH value, desorption solvent, ionic strength in sample matrix, extraction and desorption time were investigated. The results show that under the optimized experimental conditions, the method has good sensitivity, linearity, simplicity and low cost. The extraction performance of present method to the target compounds was compared with commercial SBSE which using polydimethylsiloxane as coating and other SBSEs which based on monolithic materials. The comparative results indicate that present SBSE can extract the analytes more effectively than other SBSEs because both ion-exchange and hydrophobic interactions contribute to the extraction of quinolones. 相似文献
2.
In this study, a novel stir bar sorptive extraction (SBSE) based on monolithic material (SBSEM) was prepared. The monolithic material was obtained by in situ copolymerization of vinylpyrrolidone and divinylbenzene in the presence of a porogen solvent containing cyclohexanol and 1-dodecanol with azobisisobutyronitrile as initiator. The influences of polymerization conditions on the extraction efficiencies were investigated, using phenol and p-nitrophenol as detected solutes. The monolithic material was characterized by various techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, infrared spectroscopy. Polycyclic aromatic hydrocarbons were used to investigate the extraction efficiencies of SBSEM for apolar analytes. Hormones, aromatic amines and phenols were selected as test analytes to investigate the extraction efficiencies of SBSEM for weakly and strongly polar compounds. The results showed that the new SBSEM could enrich the above-mentioned organic compounds effectively. It is worthy to mention that the SBSEM can enrich some heavy metal ions, such as Cu2+, Pb2+, Cr3+ and Cd2+, through coordination adsorption. To our best knowledge, that is the first to use SBSE to enrich heavy metal ions. 相似文献
3.
Xiaojia Huang Jianbin Lin Dongxing Yuan Rongzong Hu 《Journal of chromatography. A》2009,1216(16):3508-3511
In this study, a simple and rapid method was developed for the determination of seven steroid hormones in wastewater. Sample preparation and analysis were performed by stir bar sorptive extraction (SBSE) based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material (SBSEM) combined with high-performance liquid chromatography with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated. Under the optimized experimental conditions, the method showed good linearity and repeatability, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. The extraction performance of SBSEM to the target compounds also compared with commercial SBSE which used polydimethylsiloxane as coating. Finally, the proposed method was successfully applied to the determination of the target compounds in wastewater samples. The recoveries of spiked target compounds in real samples ranged from 48.2% to 110%. 相似文献
4.
A novel anionic exchange stir bar sorptive extraction (SBSE) coating based on poly(2-(methacryloyloxy)ethyltrimethylammonium chloride-co-divinylbenzene) monolithic material for the extraction of inorganic anion was prepared. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detailed. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to investigate the extraction capacity of the new coating for inorganic anion, the new SBSE was combined with ionic chromatography with conductivity detection, Br−, NO3−, PO43− and SO42− were selected as detected solutes. Several extractive parameters, including pH value and ionic strength in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that strongly ionic strength did not favor the extraction of anlaytes. Under the optimum experimental conditions, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target anions were achieved within the range of 0.92–2.62 and 3.03–9.25 μg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect the two different trademarks of commercial purified water with satisfactory recovery in the range of 70.0–92.6%. To the best of our knowledge, this is the first to use SBSE to enrich inorganic anions. 相似文献
5.
Maryam Kaabipour Saeid Khodadoust Fatemeh Zeraatpisheh 《Journal of separation science》2020,43(5):912-919
In this work, core/shell magnetic molecularly imprinted polymer nanoparticles were synthesized for extraction and pre‐concentration of valsartan from different samples and then it was measured with high‐performance liquid chromatography. For preparation of molecularly imprinted polymer nanoparticles, Fe3O4 nanoparticles were coated with tetraethyl orthosilicate and then functionalized with 3‐(trimethoxysilyl) propyl methacrylate. In the next step, molecularly imprinted polymer nanoparticles were synthesized under reflux and distillation conditions via polymerization of methacrylic acid, valsartan (as a template), azobisisobutyronitrile and ethylene glycol dimethacrylate as cross linking. The properties of molecularly imprinted polymer nanoparticle were investigated by FTIR spectroscopy, field emission scanning electron microscopy, and X‐ray diffraction. Box‐Behnken design with the aid of desirability function was used for optimizing the effect of variables such as the amounts of molecularly imprinted polymer nanoparticles, time of sonication, pH, and volume of methanol on the extraction percentage of valsartan. According to the obtained results, the affecting variables extraction condition were set as 10 mg of adsorbent, 16 min for sonication, pH = 5.5 and 0.6 mL methanol. The obtained linear response (r2 > 0.995) was in the range of 0.005–10 µg/mL with detection limit 0.0012 µg/mLand extraction recovery was in the range of 92–95% with standard deviation less than 6% (n = 3). 相似文献
6.
In this study, a new stir bar sorptive extraction (SBSE) coating based on poly(vinylphthalimide-co-N,N'-methylenebisacrylamide) monolith (SBSE-VPMB) was prepared. The influences of the contents of monomer in polymerization mixture and the percentage of porogen solvent on the extraction performance were investigated thoroughly. Several characteristic techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy, were used to characterize the monolithic material. The analysis of oxfendazole (OFZ) and mebendazole (MBZ) in milk and honey samples by the combination of SBSE with HPLC with diode array detection was selected as paradigms for the practical evaluation of the new coating. Under the optimized extraction conditions, the limits of detection (S/N=3) for OFZ and MBZ were 0.23-0.60 μg/L in milk and 0.24-1.08 μg/L in honey, respectively. The method also showed good linearity, repeatability, high feasibility and acceptable recoveries for real samples. At the same time, the extraction performance and the distribution coefficients (K(VPMB/W)) of OFZ and MBZ on SBSE-VPMB were compared with other SBSEs based on porous monoliths and commercial SBSE. 相似文献
7.
Multiwalled‐carbon‐nanotubes‐based matrix solid‐phase dispersion extraction coupled with high‐performance liquid chromatography for the determination of honokiol and magnolol in Magnoliae Cortex 下载免费PDF全文
Qi Zhang Bo Hong Jianhua Liu Guangze Mu Huan Cong Gang Li Defu Cai 《Journal of separation science》2014,37(11):1330-1336
In this paper, multiwalled‐carbon‐nanotube‐based matrix solid‐phase dispersion coupled to HPLC with diode array detection was used to extract and determine honokiol and magnolol from Magnoliae Cortex. The extraction efficiency of the multiwalled‐carbon‐nanotube‐based matrix solid‐phase dispersion was studied and optimized as a function of the amount of dispersing sorbent, volume of elution solvent, and flow rate of elution solvent, with the aid of response surface methodology. An amount of 0.06 g of carboxyl‐modified multiwalled carbon nanotubes and 1.5 mL of methanol at a flow rate of 1.1 mL/min were selected. The method obtained good linearity (r2 > 0.9992) and precision (RSD < 4.7%) for honokiol and magnolol, with limits of detection of 0.045 and 0.087 μg/mL, respectively. The recoveries obtained from analyzing in triplicate spiked samples were determined to be from 90.23 to 101.10% and the RSDs from 3.5 to 4.8%. The proposed method that required less samples and reagents was simpler and faster than Soxhlet and maceration extraction methods. The optimized method was applied for analyzing five real samples collected from different cultivated areas. 相似文献
8.
Peter Krajnc Dejan tefanec Jane F. Brown Neil R. Cameron 《Journal of polymer science. Part A, Polymer chemistry》2005,43(2):296-303
Water‐in‐oil high‐internal‐phase emulsions (HIPEs), containing 4‐nitrophenyl acrylate and 2,4,6‐trichlorophenyl acrylate as reactive monomers, were prepared and polymerized, and highly porous monolithic materials resulted. The novel materials were studied by combustion analysis, Fourier transform infrared spectroscopy scanning electron microscopy, mercury porosimetry, and N2 adsorption/desorption analysis. With both esters, cellular macroporous monolithic polymers were obtained; the use of 4‐nitrophenyl acrylate resulted in a cellular material with void diameters between 3 and 7 μm and approximately 3‐μm interconnects, whereas the use of 2,4,6‐trichlorophenyl acrylate yielded a foam with void diameters between 2 and 5 μm, most interconnects being around 1 μm. The resulting monoliths proved to be very reactive toward nucleophiles, and possibilities of functionalizing the novel polymer supports were demonstrated via reactions with amines bearing additional functional groups and via the synthesis of an acid chloride derivative. Tris(hydroxymethyl)aminomethane and tris(2‐aminoethyl)amine derivatives were obtained. The hydrolysis of 4‐nitrophenylacrylate removed the nitrophenyl group, yielding a monolithic acrylic acid polymer. Furthermore, functionalization to immobilized acid chloride was performed very efficiently, with more than 95% of the acid groups reacting. The measurement of the nitrogen content in 4‐nitrophenyl acrylate poly(HIPE)s after various times of hydrolysis showed the influence of the total pore volume of the monolithic polymers on the velocity of the reaction, which was faster with the more porous polymer. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 296–303, 2005 相似文献
9.
A monolithic polymer column with mixed-mode interaction was prepared by in situ polymerization in a 1000μL pipette.Two kinds of monomers,butyl methacrylate(BMA) and 2-(dimethylamino)ethyl methacrylate(DMAM) were applied to constructing the mixed-mode interaction of monolithic polymer column.Its solid-phase extraction properties for liquiritigenin(LQG) were evaluated by high performance liquid chromatography(HPLC) with a gradient elution procedure.After the extraction procedure was optimized,the maximum binding capacity and extraction recovery following the optimal extraction procedure were investigated.Calibration curve was expressed as A = 65.9C + 4.53(r~2 = 0.998) with a linear range of 0.151-1.80μg/mL.The experimental results indicate that the monolithic polymer pipette presents good extraction efficiency for LQG.It can be envisaged that the developed monolithic polymer pipette possesses the potential for its application to the enrichment of other flavonoids compounds being similar to the structure of LQG. 相似文献
10.
Xiaoli Wu Jie Liu Jinhua Wu Yang Wang Cheng Xue Ruoyu Wang Junli Hong Xuemin Zhou 《Journal of separation science》2012,35(24):3593-3599
A novel molecularly imprinted polymers (MIPs) coated micro‐stir bar (MSB) for Glibenclamide (GM) was developed. The MIPs, with GM as template molecular and methacrylic acid as functional monomer, were synthesized at the surface of the silylated MSB that was filled with magnetic core as substrate. Computational simulation was used for the optimal selection of functional monomers and porogen. The thickness of MIPs coating for MSB was about 10 μm, the adsorption and desorption time were about 40 and 20 min, respectively. The MIPs coated MSB possessed mechanical stability, high adsorption capacity, and good selectivity for GM. To achieve the optimum extraction performance, several parameters including extraction and desorption time, stirring rate, extraction and desorption solvent were investigated. A method for the determination of GM in herbal dietary supplements by MIPs coated MSB coupled with HPLC‐UV was established. The results exhibited good linear ranges of 10–6250 μg L?1 with the low limit of detection of GM (3.05 μg L?1) and the good recoveries (81.9–101.4%). 相似文献
11.
Development of a new stir bar sorptive extraction method for the determination of medium‐level volatile thiols in wine 下载免费PDF全文
Decibel Elpa Enrique Durán‐Guerrero Remedios Castro Ramón Natera Carmelo G. Barroso 《Journal of separation science》2014,37(14):1867-1872
A fast, simple, and reliable analytical method for the determination of medium‐level volatile thiols in wines is presented. Stir bar sorptive extraction using ethylene glycol‐silicone coated stir bars has been used in combination with thermal desorption gas chromatography with mass spectrometry for the analysis of 4‐mercapto‐4‐methylpentan‐2‐one, 2‐furanmethanethiol, 3‐mercaptohexyl acetate, and 3‐mercaptohexanol in wine. Optimization of the extraction technique was performed using a two‐level fractional factorial design. For the extraction step, the optimum conditions were: Ethylene glycol and silicone coated stir bars, pH at 3.5, sample volume of 25 mL, extraction time of 90 min, NaCl content 4.0 g, and stirring speed at 500 rpm. The optimized method achieved good linearity for all studied compounds (r2 > 0.995) and it provided detection limits of 21.52, 0.36, 0.73, and 2.55 μg/L for 4‐mercapto‐4‐methylpentan‐2‐one, 2‐furanmethanethiol, 3‐mercaptohexyl acetate, and 3‐mercaptohexanol, respectively. It was repeatable, with precisions lower than 18% relative standard deviation for both intraday and interday repeatability. The developed procedure is suitable for the determination of these kinds of compounds when they are present at medium concentration levels. It was finally applied to real wine samples with negative aroma derived from the high concentration levels of these compounds. 相似文献
12.
Zahra Ayazi Mehri Pourvali Amir Abbas Matin 《International journal of environmental analytical chemistry》2018,98(2):138-155
In the present work, a novel nanocomposite (NC) was prepared by reinforcing montmorillonite (MMT) into polypyrrole-nylon-6 (PPy-N6) hybrid through in situ oxidative polymerisation of PPy in the MMT-N6 mixture. The prepared novel NC was deposited as a thin layer coating on the stir bar substrate by solvent exchange method. Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray diffraction and energy dispersive X-ray spectroscopy were applied to characterise the prepared NCs. The prepared stir bar based on MMT/PPy/N6 NC was applied for sorptive extraction of some organophosphorous pesticides (OPPs) in river water samples with detection by gas chromatography-mass spectrometry (GC-MS). The effect of MMT doping level in the NC and also the effect of PPy hybridation with N6 on the coating extraction capability were studied. Central composite design was used to optimise and study the effects of influencing factors on the stir bar sorptive extraction efficiency such as salt content, pH, extraction time, desorption time, desorption solvent and its volume. The method optimisation step was performed using gas chromatography-flame ionisation detector, while the method validation was conducted using GC-MS. Limits of detection of the developed method are in the range of 0.05–0.3 μg L?1 and the linear dynamic ranges are in the range of 0.3–1000 and 1–1000 μg L?1, respectively. The intra-day precision (RSD %) of developed method with four replicates varied between 5.4 and 8.2% for distilled water spiked at 100 μg L?1. The applicability of the developed method was examined by extraction and determination of OPP compounds in river water samples, indicating the relative recoveries in the range of 80.3–95.3%. 相似文献
13.
Development and application of a polar coating for stir bar sorptive extraction of emerging pollutants from environmental water samples 总被引:1,自引:0,他引:1
In the present study, a stir bar coated with hydrophilic polymer based on poly(N-vinylpyrrolidone-co-divinylbenzene) was prepared for the sorptive extraction of polar compounds. The main parameters affecting the polymerisation of the coating were investigated.The new stir bar was applied successfully in stir bar sorptive extraction with liquid desorption followed by liquid chromatography–mass spectrometry in tandem with a triple quadrupole for the determination of a group of polar pharmaceuticals and personal care products (PPCPs) in environmental water matrices. Different variables affecting extraction and desorption such as agitation speed, temperature, ionic strength and extraction time were optimised. The results showed that the stir bar is able to enrich the selected analytes effectively.The developed method was applied to determine a group of PPCPs in different complex environmental samples, including river, effluent and influent waste water. 相似文献
14.
A simple, rapid, and sensitive method for the quantitative monitoring of five sulfonamide antibacterial residues (SAs) in milk was developed by stir bar sorptive extraction (SBSE) coupling to high performance liquid chromatography with diode array detection. The analytes were concentrated by SBSE based on poly (vinylimidazole–divinylbenzene) monolithic material as coating. The extraction procedure was very simple, milk was diluted with water then directly sorptive extraction without elimination of fats and protein in samples was required. To achieve optimum extraction performance for SAs, several parameters, including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. Under the optimized experimental conditions, low detection limits (S/N = 3) quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 1.30–7.90 ng/mL and 4.29–26.3 ng/mL from spiked milk, respectively. Good linearities were obtained for SAs with the correlation coefficients (R2) above 0.996. Finally, the proposed method was successfully applied to the determination of SAs compounds in different milk samples and satisfied recoveries of spiked target compounds in real samples were obtained. 相似文献
15.
Parezhati Pataer Turghun Muhammad Yunusjan Turahun Wenwu Yang Sailemayi Aihebaier Muyasier Wubulikasimu Lingxin Chen 《Journal of separation science》2019,42(8):1634-1643
We describe a stoichiometric approach to the synthesis of molecularly imprinted polymers specific for auramine O. Using the stoichiometric interaction in molecular imprinting, no excess of binding sites is necessary and binding sites are only located inside the imprinted cavities. The free base of the template was obtained to facilitate the interaction with the monomers. Itaconic acid was selected as the functional monomer, and stoichiometric ratio of the interaction with the free base was investigated. The molecularly imprinted polymer preparation conditions such as cross‐linker, molar ratio, porogen were optimized as divinylbenzene, 1:2:20 and chloroform/N,N‐dimethylformamide, respectively. Under the optimum conditions, a good imprinting effect and very high selectivity were achieved. A solid‐phase extraction method was developed using the molecularly imprinted polymers as a sorbent and extraction procedure was optimized. The solid‐phase extraction method showed a high extraction recovery for auramine O in its hydrochloride form and free form compared to its analogues. The results strongly indicated that stoichiometric imprinting is an efficient method for development of high selectivity molecularly imprinted polymers for auramine O. 相似文献
16.
Xiaojia Huang Ningning QiuDongxing Yuan Qingmei Lin 《Journal of chromatography. A》2009,1216(20):4354-4360
A simple and sensitive method for the determination of polar aromatic amines (PAAs) was developed using stir bar sorptive extraction (SBSE) coupling to high-performance liquid chromatography. A hydrophilic poly(vinylimidazole-divinylbenzene) (VIDB) monolithic material was prepared and acted as SBSE coating. The influences of polymerization conditions for VIDB on the extraction efficiency were investigated using aniline and 2,4-dinitroaniline as detected solutes. To achieve optimum extraction performance for PAAs, several parameters including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. The results showed that under the optimized experimental conditions, the method showed good sensitivity and excellent recoveries, as well as advantages such as linearity, simplicity, low cost and high feasibility. The extraction performance of present method to the target compounds also compared with commercial SBSE which using polydimethylsiloxane as coating and other SBSE which based on monolithic materials. Finally, the proposed method was successfully applied to the determination of PAAs in lake and sea waters, and excellent recoveries of spiked target compounds in real samples were obtained. 相似文献
17.
Preparation of a novel molecularly imprinted polymer for the highly selective extraction of baicalin 下载免费PDF全文
The selective extraction of baicalin is important to its quality control especially when the matrices are complicated. In this work, a novel molecularly imprinted polymer was prepared for the selective extraction of baicalin in herbs. The molecularly imprinted polymer was synthesized by the copolymerization of 4‐vinyl pyridine and ethylene glycol dimethacrylate in the presence of baicalin by a precipitation polymerization method. After the optimization of parameters for molecularly imprinted polymer preparation, including the functional monomer, porogen, sampling solvent, and washing solvent, good selectivity was obtained, with an imprinting factor of about 4, which is much better than that achieved by the bulk‐polymerization method. The performances of the prepared molecularly imprinted polymers were systematically investigated, including adsorption kinetics, isotherm experiment, and Scatchard analysis. On the basis of the good adsorptive capability of the prepared molecularly imprinted polymer, it was also applied for the pretreatment of baicalin in Scutellaria baicalensis Georgi. The result showed that most of the matrices were removed and baicalin was selectively enriched. 相似文献
18.
Microwave‐assisted extraction and high‐throughput monolithic‐polymer‐based micro‐solid‐phase extraction of organophosphorus,triazole, and organochlorine residues in apple 下载免费PDF全文
Habib Bagheri Ali Es'haghi Ali Es‐haghi Fatemeh Basiripour 《Journal of separation science》2016,39(3):576-583
A high‐throughput micro‐solid‐phase extraction device based on a 96‐well plate was constructed and applied to the determination of pesticide residues in various apple samples. Butyl methacrylate and ethylene glycol dimethacrylate were copolymerized as a monolithic polymer and placed in the cylindrically shaped stainless‐steel meshes of 96‐micro‐solid‐phase extraction device and used as an extracting unit. Before the micro‐solid‐phase extraction, microwave‐assisted extraction was employed to facilitate the transfer of the pesticide residues from the apple matrix to liquid media. Then, 1 mL of the aquatic samples was transferred into the 96‐well plate and the 96‐micro‐solid‐phase extraction device was applied for the extraction of the selected pesticides. Influential parameters, such as sorbent‐to‐sorbent reproducibility, microwave‐assisted extraction time, ionic strength and micro‐solid‐phase extraction time, were optimized. The limits of quantitation were below 120 μg/kg, which are lower than the maximum residue limits. The developed method was successfully implemented for the extraction and determination of the selected pesticides from 20 different apple samples gathered from local markets. Phosalone was identified and quantified at the concentration level of 147 (±16.4) μg/kg in one of the samples. 相似文献
19.
Evaluation of a method for the simultaneous quantification of N‐nitrosamines in water samples based on stir bar sorptive extraction combined with high‐performance liquid chromatography and diode array detection 下载免费PDF全文
Zahra Talebpour Simindokht Rostami Hassan Rezadoost 《Journal of separation science》2015,38(9):1601-1609
A simple, sensitive, and reliable procedure based on stir bar sorptive extraction coupled with high‐performance liquid chromatography was applied to simultaneously extract and determine three semipolar nitrosamines including N‐nitrosodibutylamine, N‐nitrosodiphenylamine, and N‐nitrosodicyclohexylamine. To achieve the optimum conditions, the effective parameters on the extraction efficiency including desorption solvent and time, ionic strength of sample, extraction time, and sample volume were systematically investigated. The optimized extraction procedure was carried out by stir bars coated with polydimethylsiloxane. Under optimum extraction conditions, the performance of the proposed method was studied. The linear dynamic range was obtained in the range of 0.95–1000 ng/mL (r = 0.9995), 0.26–1000 ng/mL (r = 0.9988) and both 0.32–100 ng/mL (r = 0.9999) and 100–1000 ng/mL (r = 0.9998) with limits of detection of 0.28, 0.08, and 0.09 ng/mL for N‐nitrosodibutylamine, N‐nitrosodiphenylamine, and N‐nitrosodicyclohexylamine, respectively. The average recoveries were obtained >81%, and the reproducibility of the proposed method presented as intra‐ and interday precision were also found with a relative standard deviation <6%. Finally, the proposed method was successfully applied to the determination of trace amounts of selected nitrosamines in various water and wastewater samples and the obtained results were confirmed using mass spectrometry. 相似文献
20.
Aixia Wei Turghun Muhammad Sailemayi Aihebaier Imran Muhammad Beibei Wu Jing Ge Amatjan Ayupbek 《Journal of separation science》2020,43(5):936-945
Glucocorticoids have a certain whitening effect on the skin. However, frequent and long‐term use of cosmetics including glucocorticoids is harmful to health. Herein, we proposed a novel micro‐solid phase extraction method for the detection of prednisolone acetate, prednisone, and prednisolone in cosmetics coupled with high‐performance liquid chromatography. In this method, porous monolithic polymer micro‐extraction bars were prepared by “one‐step, one‐pot” in situ photopolymerization combined with sacrificial support in hollow fiber under water atmosphere. The crucial factors such as pH of sample solution, extraction, and elution times that influence micro‐extraction were optimized and found to be 9.0, 2 h, and 32 min, respectively. Under the optimum experimental conditions, the linear range of the calibration curves were from 5.0 to 2000 µg/L with correlation coefficients (R2) between 0.9922 and 0.9996. The limit of detection and limit of quantification were 1.5 µg/L and 5.0 µg/L, respectively, and the recoveries were found to be in range of 69.0–113.3%. The analysis of precision for intraday and interday were less than 10.40 and 10.59%. The device has been successfully achieved photopolymerization under water atmosphere. The results indicated that this method is simple, accurate, and satisfactory for the pretreatment and determination of glucocorticoids in complex cosmetics samples. 相似文献