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ELECTROPHORESIS · 2012 ·Vol. 34 ·期 2 ·277-283 · IF 3.303

Application of ionic liquid as additive in determination of three β-agonists by capillary electrophoresis with amperometric detection

Libo Li,Hongwei Du,Huan Yu,Lei Xu,Tianyan You

CE coupled with amperometric detection method was developed using ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate (EMImBF 4 ) as additive for the simultaneous detection of clenbuterol (CLB), terbutaline (TER), and ractopamine (RAC) in feed. The effects of detection potential, concentration of EMImBF 4 , pH, and concentration of the running buffer, separation voltage as well as injection time on the separation and detection of these three β -agonists were investigated in detail. Under the optimum conditions: the detection potential at 1.05 V, 50 mmol/L Tris-HAc at pH 8.0 with 0.6% (v/v) EMImBF 4 , electrokinetic injection 6 s at 16 kV and separation voltage at 16 kV, a baseline separation for these three analytes could be achieved within 11 min. Introduction of EMImBF 4 into the running buffer resulted in significant improvement in separation selectivity and enhancement in peak currents for those β -agonists, especially for TER and RAC, which could not be separated in the running buffer without additive. The method exhibited wide linear range with LOD (S/N = 3) of 2, 1, and 2 nmol/L for CLB, TER, and RAC, respectively. The precision was determined in both intraday ( n = 5) and interday ( n = 3) assays, and the RSDs for both migration time and peak current were less than 6%. The proposed method was also applied to analyze β -agonists in feed sample.

CAS / MDL: 143314-16-3
研究领域: 分析化学 · 兽医药理学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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Analytical Methods · 2014 ·Vol. 6 ·期 24 ·9684-9690 · IF 1.938

Chemiluminescence diminishment on a paper-based analytical device: high throughput determination of β-agonists in swine hair

Xu Chen,Yong Luo,Bo Shi,Xianming Liu,Zhigang Gao,Yuguang Du,Weijie Zhao,Bingcheng Lin

β-Agonists are a group of illegal but widely used feed additives in the stockbreeding industry. In order to achieve simple-to-use, fast and high-throughput testing of this banned chemical, herein we suggest a paper-based analytical device on which a chemiluminescence diminishment method was performed. In this approach, extracts from swine hair samples as well as luminescent reagents, such as luminol and potassium periodate solution, in a low volume were applied to our device. It was found that the light emission was diminished by the β-agonists extracted from the swine hair samples. The degree of diminishment is proportional to the concentration of the β-agonists from 1.0 × 10−5 to 1.0 × 10−8 mol L−1. Also, the concentrations of solutions for chemiluminescence were optimized. The mechanism and reaction kinetics of chemiluminescence were discussed as well. The detection limit was obtained as 1.0 × 10−9 mol L−1, and recoveries from 96% to 110% were achieved, both of which suggested that our method will be favourable in field applications for swine hair samples.

CAS / MDL: 521-31-3
研究领域: 分析化学 · 兽医学 · 食品安全
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ACS Food Science & Technology · 2022 · IF 0

Determination of 18 β-Agonists in Aquatic Products Using High-Performance Liquid Chromatography Tandem Mass Spectrometry

Feng Han,Qing-ping Chen,Guangxin Yang,Wenlei Zhai,Essy Kouadio Fodjo,Liang-liang Tian,Hui-juan Yu,Yong-fu Shi,Cong Kong

An effective and efficient method for the determination of 18 β-agonists in aquatic products using liquid chromatography tandem mass spectrometry (LC-MS/MS) was successfully established. The method optimization was conducted based on incurred samples to guarantee its practicability. In this method, the sample was hydrolyzed with β-glucuronidase-arylsulfatase in ammonium acetate solution and treated successively with protein precipitation in 5% trichloroacetic acid in water, lipid removal with n-hexane, and further concentration and cleanup by solid-phase extraction (hydrophilic–lipophilic balanced cartridge, primary–secondary amine cartridge). Isotope-labeled internal standards and matrix-matched calibration curves were used for quantification. The limit of quantification (LOQ) was verified at 0.5–1.0 μg/kg (S/N > 10). This method was evaluated with five different matrices, including eel, roasted eel, pufferfish, shrimp, and crab, at 1×, 2×, and 10× LOQs, with good recoveries (>77%) and high replicate repeatability (relative standard deviations (RSDs) <13%, intraday batch repeatability) and further validated by three other accredited laboratories. A total of 3 samples out of 37 tested aquatic products were found positive for unknown incur sources (ractopamine, 0.38–2.1 μg/kg; salbutamol 3.0 μg/kg; tulobuterol 2.9 μg/kg; clenbuterol 1.3 μg/kg; and clenpenterol, 0.3 μg/kg). The method has demonstrated to be reliable, sensitive, and stable for multiresidue screening of β-agonists for food safety monitoring.

研究领域: 分析化学 · 食品安全检测
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Analytical Methods · 2020 ·Vol. 12 ·期 18 ·2317-2322 · IF 2.596

A novel microfluidic paper-based analytical device based on chemiluminescence for the determination of β-agonists in swine hair

Wei Li,Yong Luo,Xiqing Yue,Junrui Wu,Rina Wu,Yu Qiao,Qing Peng,Bo Shi,Bingcheng Lin,Xu Chen

β-Agonists are illegal feed additives in the feed industries of many countries, especially China. Here, we report a microfluidic paper-based analytical device (μPAD) coupled with the chemiluminescence (CL) method to provide the sensitive, simple and rapid quantitative detection of β-agonists in swine hair samples. In this study, we found that the β-agonists diminished the CL generated by the reaction of K3[Fe(CN)6] and luminol on μPAD, which was different from that observed in the aqueous solution, and the degree of diminishment was proportional to the concentration of β-agonists. The possible mechanism was discussed as well. Also, this detection method showed a wide linear range (from 4.0 × 10−8 to 1.0 × 10−5 mol L−1) and low limit of detection (2.0 × 10−8 mol L−1) with a low consumption of samples and reagents. Satisfactory recovery values (from 78% to 95%) were achieved. Therefore, our μPAD CL sensor will be favorable to develop a miniaturized instrument for the on-site analysis of β-agonists in swine hair samples.

研究领域: 分析化学 · 食品安全
✓ 已验证 DOI 高影响因子
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JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES · 2016 · IF 2.687

Simultaneous determination of anabolic steroids and β-agonists in milk by QuEChERS and ultra high performance liquid chromatography tandem mass spectrometry

Hongcheng Liu,Tao Lin,Xianglei Cheng,Ning Li,Luxiang Wang,Qiwan Li

A simple, accurate and highly sensitive multiresidues method was developed for the determination of 9 anabolic steroids and 16 β-agonists in milk. Target compounds were extracted and separated by a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) method with Primary secondary amine (PSA) and Zinc oxide (ZnO) nanoparticles as adsorbents. The analytes were determined by ultra high performance liquid chromatography coupled to an electro-spray ionization tandem mass spectrometer (UHPLC–MS/MS) operating in negative/positive multiple reaction monitoring mode. The effect of QuEChERS including organic solvent, amount of ZnO nanoparticle was evaluated. Good linearity was obtained for the analytes in the concentration range of 0.1–200   μg/L with a correlation coefficients higher than 0.994. Decision limits (CCα) was from 0.007   μg/kg–0.1   μg/kg, and detection capabilities (CCβ) was in the range of 0.02–0.4   μg/kg. The recoveries of these compounds were between 63% and 126% at three fortified levels. Reproducibility represented by RSD was with 10% or less. The method was successfully applied to screening of real milk samples obtained from local markets and confirmation of the suspected target analytes.

研究领域: 食品科学 · 分析化学
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FOOD CHEMISTRY · 2021 · IF 7.514

Two binding epitopes modulating specificity of immunoassay for β-agonist detection: Quantitative structure–activity relationship

Lanteng Wang,Jin Wang,Ang Zhang,Xin-an Huang,Hongtao Lei

A growing number of β -agonists are illegally using for reducing animal fat deposition in animals, but the development of analytical methods always lags behind the emergence of new illegal compounds. Therefore, class specificity antibody-based immunoassays that can detect a great many β -agonists are important for timely supervision. In this study, a competitive inhibition enzyme-linked immunosorbent assay (ciELISA) based on a clenbuterol monoclonal antibody was developed to recognize 23 β -agonists and analogues. Holographic and three-dimensional quantitative structure–activity relationship (HQSAR and 3D QSAR) revealed that there are two critical binding epitopes on β -agonist hapten affecting antibody specificity, and these epitopes have been further validated using a ractopamine antibody with narrow specificity. Tert -butyl at C-2′ epitope is needed to generate class specific antibodies, and different characteristics of substituents at benzene ring epitope would adjust antibody specificity. This investigation could provide reference for future design of β -agonist haptens.

研究领域: 食品安全 · 免疫学 · 药物化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF HAZARDOUS MATERIALS · 2014 · IF 4.331

Monitoring of PAEMs and beta-agonists in urine for a small group of experimental subjects and PAEs and beta-agonists in drinking water consumed by the same subjects

Saou-Hsing Liou,Gordon C.C. Yang,Chih-Lung Wang,Yu-Han Chiu

This 5-month study contains two parts: (1) to monitor the concentrations of 11 phthalate esters metabolites (PAEMs) and two beta-agonists in human urine samples collected from a small group of consented participants including 16 females and five males; and (2) to analyze the residues of phthalate esters (PAEs) and beta-agonists in various categories of drinking water consumed by the same group of subjects. Each category of human urine and drinking water had 183 samples of its own. The analytical results showed that nine PAEMs were detected in human urine and eight PAEs were detected in drinking water samples. It was found that average concentrations of PAEMs increased as the age increased, but no significant difference between sexes. Further, using the principal component analysis, the loadings of age effect were found to be two times greater than that of gender effect in terms of four DEHP metabolites. Regarding beta-agonists of concern (i.e., ractopamine and salbutamol), they were neither detected in human urine nor drinking water samples in this study.

研究领域: 环境科学 · 毒理学 · 公共卫生
✓ 已验证 DOI PubMed 高影响因子
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MICROCHIMICA ACTA · 2019 ·Vol. 186 ·期 2 ·1-8 · IF 5.479

One-pot synthesis of SiO2@SiO2 core-shell microspheres with controllable mesopore size as a new stationary phase for fast HPLC separation of alkyl benzenes and β-agonists

Xia Hongjun,Wang Jun,Chen Gang,Liu Jiawei,Wan Guangpin,Bai Quan

Monodisperse SiO 2 @SiO 2 core-shell silica microspheres (CSSM) with enlarged mesopores perpendicular to the particles surface were prepared using a dual-templating approach. With cetyltrimethyl ammonium bromide as the template and octyltrimethyl ammonium bromide as an auxiliary chemical, the pore size can be enlarged from 2.6 to 10.6 nm. The average shell thickness can be increased from 31 nm to 97 nm by adjusting the concentrations of the surfactants under continuous addition of tetraethyl orthosilicate. After coating twice, the resulting CSSM has a uniform mesoporous shell of about 198 nm thickness and a narrow pore size distribution. The CSSM were then modified with octadecyltrichlorosilane to give a material referred to as CS-C18. It was evaluated by separating the mixture of methylbenzene (toluene), ethylbenzene, n-propylbenzene, n-butylbenzene, n-amylbenzene and hexylbenzene. The baseline separation of the six alkyl benzenes is achieved within 2 min. Compared to a commercial column of type BEH-C18, CS-C18 shows a faster and better separation even at lower back pressure. It was also applied to the fast separation of benzo[a]pyrene, salbutamol, ractopamine and clenbuterolin residues in pork samples. The high column efficiency and better reproducibility suggest that the CSSM can be used as a matrix for fast separation and analysis of several kinds of small analytes. A dual-templating approach was utilized to produce the core shell microsphere with controllable mesopore channels by using hexadecyltrimethylammonium bromide (CTAB) as the template and trioctylmethylammonium bromide (TOMAB) as an auxiliary chemical to enlarge the size of CTAB micelles.

CAS / MDL: 50-32-8
研究领域: 材料科学 · 分析化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF SEPARATION SCIENCE · 2017 ·Vol. 40 ·期 7 ·1548-1555 · IF 2.557

Preparation of a polymer monolith modified with delaminated layered double hydroxides for the microextraction of β-agonists

Yufeng Zhou,Haijiao Zheng,Jiutong Ma,Qiong Jia

In the present study, a novel poly(acrylamide- co - N -isopropylacrylamide- co -ethylene dimethacrylate) monolithic column modified with saline-modified delaminated layered double hydroxides was developed and exploited as the stationary phase in the polymer monolith microextraction of β-agonists. Transmission electron microscopy, Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and thermal gravimetric analysis with derivative thermogravimetric determination were employed to characterize the monoliths. By coupling with high-performance liquid chromatography determinations, extraction parameters affecting the extraction efficiency, including sample volume, flow rate, sample pH, eluent volume, and eluent flow rate were investigated with an orthogonal experiment design, L 16 (4 5 ). Results demonstrated that under the optimal experimental conditions, low limits of detection in the range of 0.025–0.280 ng/mL were obtained with relative standard deviations in the range of 4.3–7.6% (intraday) and 6.7–8.8% (interday). When the developed method was applied to the analysis of β-agonists in pork samples, recovery values were obtained in the range of 80.5−108.6%.

研究领域: 分析化学 · 药物分析 · 材料科学
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JOURNAL OF CHROMATOGRAPHY A · 2024 · IF 3.8

Synthesis of polyethylene glycol-grafted magnetic nanoparticles for the fast and efficient extraction of anabolic substances from human urine

Xiaobin Zhang,Suling Zhang,Ting Lü,Wenfei Huang,Hongting Zhao,Hui Wang,Dong Zhang,Weixuan Yao

Anabolic steroids and β-agonists are commonly prohibited substances found in doping control studies; therefore, the determination of anabolic substances in biological samples is crucial. To analyze the anabolic compounds in urine, an adsorbent, polyethylene glycol (PEG)-grafted magnetic nanoparticle material (Fe 3 O 4 @SiO 2 -PEG), with low toxicity and strong biocompatibility was prepared in this investigation. Compared to those of Fe 3 O 4 and Fe 3 O 4 @SiO 2 , the grafted PEG chains (approximately 5.4 wt.%) on the magnetic nanoparticles improved the extraction efficiencies by factors of 3.9–17.0 and 2.5–2.9, respectively, likely due to the electrostatic attraction and hydrogen bonding. To achieve maximum extraction efficiency, several extraction parameters were optimized, including the kind and volume of desorption solvent, pH, and the extraction and desorption time. The standard curves were linear within the range of 0.5–20 μg/L for methyltestosterone and trenbolone, and 0.02–5 μg/L for clenbuterol. The limits of detection for the three drugs were 0.01–0.12 μg/L. The limits of quantification were 0.02–0.40 μg/L. The levels of precision of the optimized method were assessed based on the respective intra- and inter-day and batch-to-batch relative standard deviations in the ranges of 3.2–5.2 % ( n = 5), 5.9–11.3 % ( n = 4), and 6.7–9.2 % ( n = 3). The Fe 3 O 4 @SiO 2 -PEG nanoparticles could exclude urine matrix interferences (matrix effect of 91.8–98.1 %) and achieve satisfactory recoveries (75.5–116.1 %), affording sensitive and accurate determination of trace anabolic substances in urine.

研究领域: 分析化学 · 药物分析 · 生物医学工程
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Journal of Analytical Methods in Chemistry · 2018 · IF 1.262

Determination of β-Agonist Residues in Animal-Derived Food by a Liquid Chromatography-Tandem Mass Spectrometric Method Combined with Molecularly Imprinted Stir Bar Sorptive Extraction

Jiwang Tang,Jianxiu Wang,Shuyun Shi,Shengqiang Hu,Liejiang Yuan

A novel clenbuterol molecularly imprinted polymer (MIP)-coated stir bar was prepared and applied to the determination of six β-agonists in animal-derived food. Characterization and various parameters affecting adsorption and desorption behaviours were investigated. The extraction capacities of clenbuterol, salbutamol, ractopamine, mabuterol, brombuterol, and terbutaline for MIP coating were 3.8, 2.9, 3.1, 3.5, 3.2, and 3.3 times higher, respectively, than those of the NIP coating, respectively. The method of MIP-coated SBSE coupled with HPLC-MS/MS was developed. The recoveries in pork and liver samples were 75.8–97.9% with RSD from 2.6 to 5.3%. Limits of detection (LODs) and limits of quantification (LOQs) were 0.05–0.15 μg/kg and 0.10–0.30 μg/kg, respectively. Good linearities were obtained for six β-agonists with correlation coefficients (R2) higher than 0.994. These results indicated the superiority of the proposed method in the analysis of β-agonists in a complex matrix.

CAS / MDL: 97-90-5
研究领域: 分析化学 · 食品安全
✓ 已验证 产品关联 DOI PubMed 高影响因子
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ACTA PHARMACOLOGICA SINICA · 2024 · IF 6.9

A new mechanism of thyroid hormone receptor β agonists ameliorating nonalcoholic steatohepatitis by inhibiting intestinal lipid absorption via remodeling bile acid profiles

Sun Kai,Zhu Nan-lin,Huang Su-ling,Qu Hui,Gu Yi-pei,Qin Li,Liu Jia,Leng Ying

Excessive dietary calories lead to systemic metabolic disorders, disturb hepatic lipid metabolism, and aggravate nonalcoholic steatohepatitis (NASH). Bile acids (BAs) play key roles in regulating nutrition absorption and systemic energy homeostasis. Resmetirom is a selective thyroid hormone receptor β (THRβ) agonist and the first approved drug for NASH treatment. It is well known that the THRβ activation could promote intrahepatic lipid catabolism and improve mitochondrial function, however, its effects on intestinal lipid absorption and BA compositions remain unknown. In the present study, the choline-deficient, L -amino acid defined, high-fat diet (CDAHFD) and high-fat diet plus CCl 4 (HFD+CCl 4 )-induced NASH mice were used to evaluate the effects of resmetirom on lipid and BA composition. We showed that resmetirom administration (10 mg·kg −1 ·d −1 , i.g.) significantly altered hepatic lipid composition, especially reduced the C18:2 fatty acyl chain-containing triglyceride (TG) and phosphatidylcholine (PC) in the two NASH mouse models, suggesting that THRβ activation inhibited intestinal lipid absorption since C18:2 fatty acid could be obtained only from diet. Targeted analysis of BAs showed that resmetirom treatment markedly reduced the hepatic and intestinal 12-OH to non-12-OH BAs ratio by suppressing cytochrome P450 8B1 (CYP8B1) expression in both NASH mouse models. The direct inhibition by resmetirom on intestinal lipid absorption was further verified by the BODIPY gavage and the oral fat tolerance test. In addition, disturbance of the altered BA profiles by exogenous cholic acid (CA) supplementation abolished the inhibitory effects of resmetirom on intestinal lipid absorption in both normal and CDAHFD-fed mice, suggesting that resmetirom inhibited intestinal lipid absorption by reducing 12-OH BAs content. In conclusion, we discovered a novel mechanism of THRβ agonists on NASH treatment by inhibiting intestinal lipid absorption through remodeling BAs composition, which highlights the multiple regulation of THRβ activation on lipid metabolism and extends the current knowledge on the action mechanisms of THRβ agonists in NASH treatment.

CAS / MDL: 56-23-5 8001-25-0
研究领域: 代谢生物学 · 肝脏病学 · 药理学
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