Two-dimensional hydrophilic imprinted resin-graphene oxide composite for selective extraction and rapid determination of gibberellin traces in licorice samples.

This study presents novel methodologies and materials for selectively and sensitively determining gibberellin traces in licorice to address food safety concerns. A novel hydrophilic imprinted resin-graphene oxide composite (HMIR-GO) was developed with fast mass transfer, high adsorption capacity, and exceptional aqueous recognition performance for gibberellin. Leveraging the advantages of molecular imprinting, hydrophilic resin synthesis, and rapid mass transfer characteristics of GO, HMIR-GO was employed as an adsorbent, showing resistance to matrix interference. Coupled with HPLC, a rapid and selective method for determining gibberellin was established. Under optimal conditions, the method exhibited a wide linear range (0.02-5.00 µg g-1, r = 0.9999), low detection limits (3.3 ng g-1), and satisfactory recoveries (92.0-98.4%), enabling the accurate and rapid detection of gibberellin in licorice. This study introduces a pioneering strategy for the selective extraction and determination of trace gibberellin levels, offering insights for similar applications in functional foods.

Preparation of poly (methacrylic acid)/graphene oxide aerogel as solid-phase extraction adsorbent for extraction and determination of dopamine and tyrosine in urine of patients with depression.

Dopamine (DA) and l-tyrosine (l-Tyr) are neurotransmitters involved in various neuropsychiatric disorders. Therefore, it is important to monitor their levels for diagnosis and treatment. In this study, we synthesized poly (methacrylic acid)/graphene oxide aerogels (p(MAA)/GOA) by in situ polymerization and freeze-drying using graphene oxide and methacrylic acid as substrates. Then, the p(MAA)/GOA were applied as solid-phase extraction adsorbents to extract DA and l-Tyr from urine samples, followed by quantification using high performance liquid chromatography (HPLC). The p(MAA)/GOA showed better adsorption performance for DA and l-Tyr than commercial adsorbents, likely as a result of the strong adsorption of the target analytes via π-π and hydrogen bonding interactions. Further, the developed method had good linearity (r > 0.9990) at concentrations of DA and l-Tyr of 0.075-2.0 and 0.75-20.0 µg mL-1, respectively, as well as a limit of detection of 0.018-0.048 µg mL-1, limit of quantitation of 0.059-0.161 µg mL-1, spiked recovery of 91.1-104.0%, and interday precision of 3.58-7.30%.The method was successfully applied to determine DA and l-Tyr in the urine samples of patients suffering from depression, demonstrating its potential for clinical applications.

Fabrication of superparamagnetic bovine haemoglobin surface-imprinted core-shell nanocomposite adsorbent via emulsion-free sol-gel polymerization.

A new strategy has been developed to fabricate a bovine haemoglobin surface-imprinted core-shell nanocomposite adsorbent, demonstrating superparamagnetism via emulsion-free and sol-gel techniques. The obtained magnetic surface-imprinted polymers (MSIPs) possess a porous core-shell nanocomposite structure with a remarkable imprinted recognition ability for template protein in aqueous medium. The MSIPs display higher affinity, adsorption efficiency and selectivity, for template protein compared to the non-target protein. The morphology, adsorption, and recognition properties of the MSIPs have been evaluated by using several characterisation techniques, such as scanning electron microscopy, transmission electron microscopy, X-ray powder diffraction, Fourier transform infrared spectroscopy, thermogravimetric analysis, and vibrating sample magnetometry. The results show the average diameter of MSIPs ranging between 400 and 600 nm with a saturation magnetization value of 52.6 emu/g and adsorption capacity of 43.75 mg/g. And because the obtained MSIPs possessed easily accessible recognition sites and performed fast kinetics for template immobilization, it could achieve equilibrium within 60 min. All this revealed the potential application of this approach as an alternative methodology for the generation of protein imprinted biomaterials.

Dual-template hydrophilic imprinted resin as an adsorbent for highly selective simultaneous extraction and determination of multiple trace plant growth regulators in red wine samples.

In recent years, numerous plant growth regulators have been found in foods and have a toxicity to human health, so its simultaneous multiple monitoring is urgently. For the first time, a rapid, accurate, and high-selective method was established to extract and determine multiple plant growth regulators simultaneously in red wines using a new dual-template hydrophilic molecularly imprinted resin (DHMIR) as an adsorbent of pipette tip solid-phase extraction coupled with HPLC. The as-prepared DHMIR combined the advantages of the hydrophilicity of hydrophilic resin and multi-imprinted recognition of dual-template molecular imprinting, overcoming the poor imprinted recognition ability of traditional imprinting materials in water and low extraction efficiency to multiple targets. Under the optimized conditions, the proposed method exhibited high sensitivity (2.29-3.94 ng mL-1) and recoveries (80.9-109.0 %) using only 15 mg DHMIR. This study provides an effective strategy for rapid, accurate, low-cost, and high-selective determination of the multiple analytes in food samples.

Novel molecularly imprinted phenolic resin-dispersive filter extraction for rapid determination of perfluorooctanoic acid and perfluorooctane sulfonate in milk.

Perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) are emerging pollutants that threaten food safety. Herein, a rapid, accurate, and selective method for determination of PFOA and PFOS in milk was established by using new molecularly imprinted phenolic resin (MIP-PR) as the adsorbent of dispersive filter extraction (DFE) combined with liquid chromatography-tandem mass spectrometry (LC-MS/MS). MIP-PR was synthesized at room-temperature using m-aminophenol, glutaraldehyde, and perfluorononanoic acid as the monomers, cross-linkers, and virtual templates, respectively, and exhibited rapid mass transfer (30 s), high selectivity (imprinted factors > 3.7), and large adsorption capacity (>54.6 mg/g). Compared with reported methods, the developed MIP-PR-DFE method is fast, selective, inexpensive, and shows good purification and enrichment efficiency. The proposed MIP-PR-DFE-LC-MS/MS exhibited low limits of detection (0.006-0.022 ng/mL), high recoveries (94.7-109 %), and good precision (RSDs ≤ 9.5 %). This study provides a new idea for the development of imprinted resin adsorbents for perfluorinated compound, and a new method for sample pretreatment for monitoring of PFOA and PFOS in food.

Miniaturized extraction and determination of swelling agents in fruits and vegetables based on deep eutectic solvent-molecularly imprinted hydrophilic resin.

The overuse of swelling agents in fruits and vegetables has rapidly increased, resulting in food safety problems. Hence, a new method for the selective extraction and detection of thidiazuron (TDZ) and forchlorfenuron (KT30) was developed using deep eutectic solvent-molecularly imprinted hydrophilic resin (DES-MIHR) as a pipette tip solid-phase extraction (PT-SPE) adsorbent with excellent molecular recognition in aqueous matrixes. DES-MIHR interacted with TDZ and KT30 via π-π interactions and hydrogen bonding. The miniaturized PT-SPE can be performed with just 5.0 mg adsorbent, 0.3 mL water, and 0.2 mL eluent, thus having the advantage of the low consumption of adsorbent and organic reagents. The performance of the DES-MIHR-PT-SPE-high-performance liquid chromatography (HPLC) method was demonstrated with the recoveries from various fruits and vegetables being 81.1-102.9 % (RSD ≤ 7.1 %). Thereby indicating the general applicability of the developed method for the accurate determination of trace swelling agents in fruits and vegetables.

Analysis of anticancer compound, indole-3-carbinol, in broccoli using a new ultrasound-assisted dispersive-filter extraction method based on poly(deep eutectic solvent)-graphene oxide nanocomposite.

Indole-3-carbinol (I3C), an important anticancer compound found in broccoli, has attracted considerable attention. The rapid extraction and accurate analysis of I3C in the pharmaceutical industry in broccoli is challenging as I3C is unstable at low pH and high temperature. In this study, a rapid, accurate, and low-cost ultrasound-assisted dispersive-filter extraction (UADFE) technique based on poly(deep eutectic solvent)-graphene oxide (PDES-GO) adsorbent was developed for the isolation and analysis of I3C in broccoli for the first time. PDES-GO with multiple adsorption interactions and a fast mass transfer rate was synthesized to accelerate adsorption and desorption. UADFE was developed by combining dispersive solid-phase extraction (DSPE) and filter solid-phase extraction (FSPE) to realize rapid extraction and separation. Based on the above two strategies, the proposed PDES-GO-UADFE method coupled with high-performance liquid chromatography (HPLC) allowed the rapid (15-16 min), accurate (84.3%-96.4%), and low-cost (adsorbent: 3.00 mg) analysis of I3C in broccoli and was superior to solid-phase extraction, DSPE, and FSPE methods. The proposed method showed remarkable linearity (r=0.9998; range: 0.0840-48.0 µg/g), low limit of quantification (0.0840 µg/g), and high precision (relative standard deviation ≤5.6%). Therefore, the PDES-GO-UADFE-HPLC method shows significant potential in the field of pharmaceutical analysis for the separation and analysis of anti-cancer compounds in complex plant samples.

Improved Solid-Phase Extraction for Simple, Sensitive, and Efficient Determination of Trace Plant Growth Regulators in Cherry Tomatoes by High-Performance Liquid Chromatography.

The overuse of plant growth regulators (PGRs) in agricultural products has gradually increased in recent years, resulting in hazardous effects on food safety and human health. For the first time, a sensitive, accurate, and low-cost analytical method involving improved solid-phase extraction coupled with high-performance liquid chromatography was developed to determine trace PGRs in cherry tomatoes. Thereafter, the extraction mechanism and conditions were elucidated. Under optimized conditions, good linearity (0.04-400 ng g-1; r ≥ 0.9996) and lower limits of detection (0.005-0.006 ng g-1) were observed. The recoveries were 81.4-90.1%, with relative standard deviations of ≤6.7% (three levels). Finally, the developed method was successfully used to detect trace PGRs in cherry tomatoes. The results illustrated that this sensitive method shows great potential for application to monitor trace PGRs in agricultural products and, thus, provide technical support for food safety and public health.

Ionic liquid-organic-functionalized ordered mesoporous silica-integrated dispersive solid-phase extraction for determination of plant growth regulators in fresh Panax ginseng.

The massive accumulation of plant growth regulators (PGRs) in Panax ginseng causes serious harm to human health. A new analytical method for the simultaneous determination of multiple PGRs in 19 types of fresh Panax ginseng is developed by a new designed wool cluster-inspired ionic liquid-functionalized ordered mesoporous silica-integrated dispersive solid-phase extraction coupled to high performance liquid chromatography (IL-WFOMS-I-DSPE-HPLC). The proposed method combines the advantages of the multiple adsorption mechanisms, high mass transfer rate and large adsorption capacity of the synthesized IL-WFOMS adsorbent with the safe, convenient operation of the new designed I-DSPE method. Under optimized conditions, the recoveries at three spike levels were in a range of 77.6-98.3% for 3-indole acetic acid (IAA), 3-indole propionic acid (IPA), 3-indole butyric acid (IBA), and 1-naphthaleneacetic acid (NAA) with the relative standard deviations (RSD) ≤8.6%, n = 3. This method exhibits the advantages of safety, convenience, reliability, and has great potential for simultaneous determination of multiple trace PGRs in complex sample matrices.

Attapulgite/hydrophilic molecularly imprinted monolithic resin composite for the selective recognition and sensitive determination of plant growth regulators in cucumbers.

In this study, through in-situ polymerization process, a novel composite of attapulgite/hydrophilic molecularly imprinted monolithic resin (AT/HMIMR) were prepared in pipette tips for extraction trace plant growth regulators in cucumbers. In the preparation procedure, fibrillar attapulgite nanoparticles were embedded to increase extraction capacity, polyethyleneglycol-6000 was employed as a dual-function porogen, that acted as both the structure-directing agent of the HMIMR and the attapulgite dispersant. N-(1-naphthyl) ethylenediamine dihydrochloride was used as a dummy template to accurate quantification on extraction procedures. Experimental parameters of AT/HMIMR for extracting plant growth regulators from cucumbers were optimized, and the results showed that the recoveries of ranged from 92.4% to 101.1% with relative standard deviations ≤ 6.5% (n = 3). Considering its microporous monolithic column structure, multiple adsorption mechanism, and specific selectivity, AT/HMIMR shows promise for applications that require specific recognition for the analytes in real complex samples.

Green protocol for the preparation of hydrophilic molecularly imprinted resin in water for the efficient selective extraction and determination of plant hormones from bean sprouts.

In this study, a novel and green synthesis of a new hydrophilic molecularly imprinted 3-aminophenol-hexamethylenetetramine (MIAPH) resin for the selective recognition and separation of plant hormones was developed. The MIAPH resin was obtained using 3-aminophenol as multifunctional monomer which introduced hydroxyl, amino, and imino groups simultaneously, and adenine was used as a dummy template for molecular imprinting. Meanwhile, hexamethylenetetramine released formaldehyde slowly through hydrolysis which was used as the cross-linking agent to avoid the direct and excessive use of toxic formaldehyde. The entire procedure was performed under mild conditions, and was facile, environmentally friendly and energy-efficient. The obtained MIAPH resin showed high specific recognition toward plant hormones and higher recoveries in bean sprouts compared to NIAPH, HLB, and C18. Various parameters affecting the extraction efficiency were optimized, and the calibration linearity of the MIAPH‒SPE‒HPLC method was determined from 0.07 to 2.86 mg kg-1 with a correlation coefficient (r) ≥ 0.9994 under the optimal conditions. Recoveries of spiked standards ranged from 90.2 to 99.1% for bean sprout with a relative standard deviation of ≤5.3%. Finally, the established MIAPH‒SPE‒HPLC method was successfully applied for the selective extraction and sensitive detection of plant hormones in a variety of complex vegetable matrices.

Green synthesis of hydrophilic protein-imprinted resin with specific recognition of bovine serum albumin in aqueous matrix.

The synthesis of biomacromolecule imprinted materials is a challenge with the bulkiness and instability of macromolecule, such as protein. A green strategy to prepare hydrophilic protein-imprinted resin (HPIR) was firstly developed using resorcinol and melamine as double functional monomers, hexamethylenetetramine instead of formaldehyde as crosslinker, water as solvent, and bovine serum albumin (BSA) as a dual-function template. BSA as dual-function template could not only act as template but also porogen in the preparation of HPIR. According to the adsorption experiments, the adsorption kinetics of BSA on HPIR obeyed pseudo-second-order adsorption kinetics and the equilibrium data were best described by Langmuir isotherm model. The adsorption capability was 44.3459 mg g-1 (25 °C), and the imprinted factor for binding BSA is 5.78. HPIR showed high adsorption capacity, fast mass transfer rate, and specific selectivity towards BSA in aqueous solvent. More importantly, HPIR can be applied to selectively adsorb target protein BSA in urine without the matrix interference of biological matrix, therefore, it is promising for HPIR to be applied to proteomics, diagnostics, and pharmaceutics.

An ionic liquid functionalized graphene adsorbent with multiple adsorption mechanisms for pipette-tip solid-phase extraction of auxins in soybean sprouts.

A new ionic liquid functionalized graphene-pipette-tip solid-phase extraction method coupled with high-performance liquid chromatography was established for the simultaneous extraction and determination of three auxins in soybean sprouts. The graphene adsorbent, with multiple adsorption mechanisms, was first synthesized by functional modification of pentafluorobenzyl imidazolium bromide ionic liquid through thiol-ene click chemistry. The ionic liquid was applied to prevent the aggregation of graphene; it also imbued graphene with the ability for π-π interactions, ionic exchange, electrostatic interactions, as well as hydrogen bonding (which is stronger than the interaction between water and analytes), by augmenting the adsorption mechanisms between the adsorbent and analytes. Under optimized conditions, linearity was achieved in the ranges 0.03-5.00 µg/g for indole-3-acetic acid and 1-naphthaleneacetic acid and 0.09-5.00 µg/g for 2,4-dichlorophenoxyacetic acid, with a detection limit of 0.004-0.026 µg/g; this adsorbent has been successfully applied for the determination of auxins in soybean sprouts.

An ionic liquid-magnetic graphene composite for magnet dispersive solid-phase extraction of triazine herbicides in surface water followed by high performance liquid chromatography.

A new ionic liquid-magnetic graphene (IL-MG) composite was used as the adsorbent in magnetic dispersive solid-phase extraction to rapidly extract and isolate triazine herbicides from surface water. IL-MG was synthesized by a simple and time-saving one-pot strategy where the synthesis of magnetic Fe3O4, the modification with an IL, and the reduction of graphene oxide to graphene were conducted at the same time. An IL was applied to enrich the interaction mechanism between IL-MG and analytes (π-π, hydrophobic interaction, and electrostatic interaction). Moreover, the IL and Fe3O4 nanoparticles acted as spacers, inserting between the layers of graphene to prevent the aggregation of graphene, which improved the adsorption ability because of the large specific surface area of IL-MG. The resultant IL-MG had hierarchical flake structures and showed a high adsorption capacity (8266.0-12 324.1 µg g-1) toward triazine herbicides. Under suitable conditions, the linearity for triazine herbicides was achieved in the range of 0.55-500 ng mL-1 with a detection limit of 0.09-0.15 ng mL-1 and a quantitation limit of 0.31-0.51 ng mL-1, and the enrichment factor was 83-fold, which indicated that the proposed method could be successfully applied for the determination of triazine herbicides in surface water.

Bifunctionalized ordered mesoporous organosilica synthesized in deep eutectic solvent for extraction of triazine herbicides from watermelon.

A C8-and-amino-bifunctionalized ordered mesoporous organosilica (C8-AMS) was prepared in a deep eutectic solvent-a green solvent-that was used as the reaction medium for this procedure instead of organic solvents or other catalyst for the first time. This method provided a nontoxic way for C8 grafting and obtaining an ordered mesoporous organosilica material with both hydrophilic and hydrophobic groups. Besides advantages such as its large surface area, regular and uniform pore size, and hydrothermal stability, the obtained bifunctionalized C8-AMS also have two main functional groups in the obtained structure, C8 and amino, which enriched the adsorption mechanism of the material and as a result improved the adsorption selectivity of C8-AMS. Its performance as an adsorbent was estimated in extracting trace triazine herbicides from watermelon using solid-phase extraction (SPE) followed by high-performance liquid chromatography (HPLC). The proposed method provided satisfactory features in terms of linearity (0.01-2.00µgg-1), limits of detection (2.9-5.1ngg-1), accuracy (recovery: 85.7-101.7%), and precision (intra-day and inter-day RSDs: 1.68-2.60% and 3.05-4.01%).

One-pot synthesis of ethylenediamine-connected graphene/carbon nanotube composite material for isolation of clenbuterol from pork.

A fluffy porous ethylenediamine-connected graphene/carbon nanotube composite (EGC), prepared by a simple and time-saving one-pot synthesis, was successfully applied as an adsorbent in pipette-tip solid-phase extraction (PT-SPE) for the rapid extraction and determination of clenbuterol (CLB) from pork. In the one-pot synthesis, carbon nanotubes were inserted into graphene sheets and then connected with ethylenediamine through chemical modification to form a three-dimensional framework structure to prevent agglomeration of the graphene sheets. Under the optimum conditions for extraction and determination, good linearity was achieved for CLB in the range of 15.0-1000.0ngg-1 (r=0.9998) and the recoveries at three spiked levels were in the range of 92.2-96.2% with relative standard deviation ≤9.2% (n=3). In comparison with other adsorbents, including silica, NH2, C18, and Al2O3, EGC showed higher extraction and purification efficiency for CLB from pork samples. This analytical method combines excellent adsorption performance of EGC and high extraction efficiency of PT-SPE.

Graphene/multi-walled carbon nanotubes functionalized with an amine-terminated ionic liquid for determination of (Z)-3-(chloromethylene)-6-fluorothiochroman-4-one in urine.

A new type of amine-terminated-ionic-liquid-functionalized graphene/multi-walled carbon nanotubes hybrid material (IL-G/MWCNTs) was synthesized and used as an adsorbent in miniaturized pipette tip solid-phase extraction (PT-SPE) coupled with liquid chromatography for the isolation and determination of (Z)-3-(chloromethylene)-6-fluorothiochroman-4-one (CMFT) in urine. Parameters for the preparation of IL-G/MWCNTs and the PT-SPE procedure, including the mass ratio of graphene oxide and oxidized multi-walled carbon nanotubes, the mass ratio of graphene oxide and the ionic liquid, and the type and volume of washing and elution solvents were optimized to achieve higher extraction efficiency. Good linearity of the method was achieved in the range 0.03-5.0µgmL-1 with a coefficient of determination (r2) of 0.9999. The limits of detection and quantification were 0.009 and 0.030µgmL-1, respectively. The intra- and inter-day precisions, expressed as relative standard deviations (RSDs), were evaluated by performing replicate analyses of samples spiked at 0.1µgmL-1 on the same day (n=6) and over three consecutive days, and were 4.8 and 5.5%, respectively. Recoveries between 73.9 and 93.9% were obtained at three spiking levels, with RSDs≤7.9%. Five batches of the adsorbent were investigated to confirm the reliability of the preparation method.

Hydrophilic molecularly imprinted melamine-urea-formaldehyde monolithic resin prepared in water for selective recognition of plant growth regulators.

New hydrophilic molecularly imprinted melamine-urea-formaldehyde monolithic resin (MIMR) is synthesized using dopamine hydrochloride as a dummy template via in-situ polymerization directly within pipette tips and it presents special molecular recognition to plant growth regulators in aqueous matrices. Hydrophilic groups (such as hydroxyl groups, imino groups, and amino groups) can be introduced into MIMR by melamine- urea-formaldehyde resin, which make MIMR materials compatible with aqueous media and show their specific molecular recognition in aqueous sample solutions. Meanwhile, monolithic structures avoid the influence of uneven filling on the extraction efficiency. Various parameters affecting the selective recognition of MIMR have been optimized, such as molar ratio of melamine to urea, molar ratio of melamine and urea to formaldehyde, the amount of template and porogen. The prepared MIMR is applied as the sorbents of solid phase extraction (SPE) for sensitive and selective recognition of three plant growth regulators (p-chlorophenoxyacetic acid, 1-naphthaleneacetic acid and 2.4-dichlorophenoxyacetic acid) in bean sprouts. Considering its excellent hydrophilicity and specificity, MIMR-SPE is promising to be a potential pretreatment strategy in biological, environmental, and clinical fields.

Water-compatible dummy molecularly imprinted resin prepared in aqueous solution for green miniaturized solid-phase extraction of plant growth regulators.

A water-compatible dummy molecularly imprinted resin (MIR) was synthesized in water using melamine, urea, and formaldehyde as hydrophilic monomers of co-polycondensation. A triblock copolymer (PEO-PPO-PEO, P123) was used as porogen to dredge the network structure of MIR, and N-(1-naphthyl) ethylenediamine dihydrochloride, which has similar shape and size to the target analytes, was the dummy template of molecular imprinting. The obtained MIR was used as the adsorbent in a green miniaturized solid-phase extraction (MIR⬜mini-SPE) of plant growth regulators, and there was no organic solvent used in the entire MIR⬜mini-SPE procedure. The calibration linearity of MIR⬜mini-SPE⬜HPLC method was obtained in a range 5⬜250ngmL(↙1) for IAA, IPA, IBA, and NAA with correlation coefficient (r) Ⱕ0.9998. Recoveries at three spike levels are in the range of 87.6⬜100.0% for coconut juice with relative standard deviations Ⱔ8.1%. The MIR⬜mini-SPE method possesses the advantages of environmental friendliness, simple operation, and high efficiency, so it is potential to apply the green pretreatment strategy to extraction of trace analytes in aqueous samples.

Synthesis of mimic molecularly imprinted ordered mesoporous silica adsorbent by thermally reversible semicovalent approach for pipette-tip solid-phase extraction-liquid chromatography fluorescence determination of estradiol in milk.

A mimic molecularly imprinted ordered mesoporous silica (MIOMS) adsorbent was prepared utilizing a thermally reversible semicovalent approach. The thermally reversible covalent template-monomer complex was firstly synthesized by employing 4,4'-sulfonyldiphenol (BPS) and (3-isocyanatopropyl) triethoxysilane (ICPTES) as template and monomer, respectively. The template-monomer complex was incorporated into ordered mesoporous silica via a simple self-assembly process. The adsorption experiment illustrated that the imprint-removed silica (MIOMS-ir) had higher special recognition ability (250µgg(-1)) for estradiol (E2) than the non-imprinted silica (NIOMS-ir) (25µgg(-1)). MIOMS-ir was applied as an adsorbent in pipette-tip solid-phase extraction (PT-SPE) coupled with liquid chromatography-fluorescence detector (LC-FLD) for determination of E2 in milk samples. Under the optimized conditions, only 3mg of the adsorbent, 0.3mL of water as washing solvent, and 0.5mL of acetonitrile-acetic acid (96:4, v/v) as elution solvent were used in the pretreatment procedure of milk samples. Good calibration linearity was obtained in a range of 25ngL(-1) to 1000ngL(-1), and the recoveries at three spiked levels were ranged from 95.4% to 107.0% with relative standard deviations (RSDs) ≤3.1% (n=3). The proposed MIOMS-ir-PT-SPE-LC-FLD method combined the advantages of PT-SPE and ordered mesoporous material such as ease assembly, low cost, high extraction efficiency and large specific surface area, so it is a potential pretreatment strategy for the extraction and determination of E2 in complex milk samples.