查找使用阿拉丁产品的科研文献

Fast Determination of Propofol in Human Plasma Using C18-Functionalized Magnetic Nanomaterials Followed by Supercritical Fluid Chromatography

Liang Shan-Yan,Xu Xiao-Min,Wang Peng,Ye Ming-Li,Zhang Shui-Feng,Zhao Yong-Gang

Novel C18-functionalized magnetic nanomaterials; i.e., C18@poly-styrene-divinylbenzene-glycidyl methacrylate-Fe3O4 (C18@PS-DVB-GMA-Fe3O4) have been synthesized by using N, N-dimethyloctadecylamine as modifying agent, which could be beneficial to remove the blood phospholipids. The C18@PS-DVB-GMA-Fe3O4 nanoparticles have been used and evaluated in the Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) procedure for human plasma prior to the analysis of propofol by supercritical fluid chromatography (SFC). In the QuEChERS procedure, human plasma samples are directly mixed with extraction solvent and C18@PS-DVB-GMA-Fe3O4 nanoparticles, and the extraction and cleanup procedures have been accomplished simultaneously. The SFC separation was performed with a C18 column (Thermo Scientific™ Acclaim™ 120, 250 × 4. 6 mm, 5 μm) within 5 min, using thymol as the internal standard. Supercritical carbon dioxide was used as the mobile phase with methanol as the cosolvent at the flow rate of 1.0 mL/min. The column temperature was 38°C, and detection wavelength was 275 nm. A good linearity was obtained among the propofol concentration range of 0.5–10 mg/L (R2 = 0.9997) with the limit of detection of 0.17 mg/L. Recoveries were in the range of 76.5–91.9%, with RSD less than 7.9%. These results suggested that method is convenient, rapid with high accuracy and little matrix effect, and suitable for rapid determination of propofol plasma concentration.

Magnetic solid-phase extraction modified Quick, Easy, Cheap, Effective, Rugged and Safe method combined with pre-column derivatization and ultra-high performance liquid chromatography-tandem mass spectrometry for determination of estrogens and estrogen mimics in pork and chicken samples

Xiang Xiong,Dan Li,Zhifeng Du,Chaomei Xiong,Hongliang Jiang

In this study, conventional Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method was modified by magnetic solid-phase extraction (MSPE) for purification/pre-concentration of eleven estrogens and estrogen mimics from the extracts of pork and chicken muscles, prior to dansyl chloride (DNS-Cl) derivatization coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) assay. Dual octadecyl- and 2-aminoethyl-3-aminopropyl- groups functionalized mesoporous silica core-shell magnetic nanoparticles (C 18 /NH 2 -Fe 3 O 4 @mSiO 2 MNPs) were synthesized and employed as MSPE sorbent with remarkable aqueous compatibility in comparison with conventional C 18 functionalized sorbent. The proposed MSPE is easier to handle than the traditional SPE purification process in QuEChERS method. The lab-prepared MNPs were characterized by transmission electron microscope (TEM), brunner-emmet-teller (BET), dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FT-IR), thermo-gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). Pre-column derivatization was conducted to significantly enhance the sensitivity of the analytes in MS/MS via analyzing their derivatives in positive ion mode instead of analyzing their original forms in negative ion mode. Under the optimal sample pretreatment and instrumental analysis conditions, the approach showed low limits of detection (LODs, 0.02‒3.00 µg kg –1 ), appropriate recoveries (81.1‒115.4%) and acceptable precisions (0.48‒15.1%, n  = 6), with good feasibility and future prospect of trace compounds analysis in complex food samples.

A modified QuEChERS method for the determination of sulfonamides in animal-derived food using enzymatic inhibition assay

Juanli Du,Shuang Feng,Wenying Wu,Xu Jing,Hao Wu,Kasim Sakran Abass,Xiaowen Wang,Jianhai Zhang

Sulfonamides (SAs) are widely used, and their residues pose a serious threat to food safety and human health. Herein, we developed a green, accurate, and sensitive method for detecting SAs residues in animal-derived food using a modified QuEChERS method combined with enzyme inhibition–based colorimetry. Magnetic COF (TpPa-Cl)@Fe 3 O 4 was simple to synthesise, chemically stable and reusable. When used as an adsorbent in modified QuEChERS, it simplifies the purification process and has a high purification capacity. An environmentally friendly natural deep eutectic solvent synthesized using propylene glycol and betaine can serve as a green substitute for traditional organic extractants. SAs were detected by inhibiting the colorimetric reaction between carbonic anhydrase and p -nitrophenyl acetate, and were quantitatively analyzed by digital image colorimetry (DIC) of smartphone. Under optimal conditions, the limits of detection and quantification were 0.53–0.86   µg·kg −1 and 1.52–1.95   µg·kg −1 , respectively. The recoveries of SAs were in the range of 93.60%–101.60%, and the relative standard deviation was < 4.9%. Based on the combined results, our developed method has good applicability in the analysis of SAs residues in food.

Simultaneous Determination of Six Acidic Herbicides and Metabolites in Plant Origin Matrices by QuEChERS-UPLC-MS/MS

Qiqi Jin,Qianwen Xu,Zhiyong Zhao,Wenshuai Si,Bing Bai,Lei Chen,Changyan Zhou

This study presents a method for the simultaneous determination of six acidic herbicides and their metabolites in various matrices, including fruits, vegetables, grains, and edible oils. The method employs acidified acetonitrile extraction combined with dispersive solid-phase extraction cleanup (dSPE) using MgSO4, Florisil, and Graphitized carbon black (GCB). The analysis was performed by ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization (ESI) in both positive and negative modes using multiple reaction monitoring (MRM). The mass concentrations of six herbicide pesticides and their metabolites were predominantly within the range of 0.0005~0.050 mg/L and exhibited strong linear relationships with the corresponding peak area, with the coefficient of determination (R2) exceeding 0.993. The limits of detection (LOD) for the method ranged from 0.0001 to 0.008 mg/kg. The recovery rates of adding recovery experiments to cabbage, chives, pear, wheat flour, and soybean oil were 69.8~120%, and the relative standard deviation (RSD) was 0.6~19.5%. The results indicate that this method is efficient and fast, and can be used for the detection of compounds in various actual matrices.

Novel magnetic nanoparticle-assisted QuEChERS-UHPLC-MS/MS for the determination of multi-mycotoxins in complex sample matrices

Ruifeng Lin,Huiqiang Feng,Zhixin Zhang,Yanling Liu,Hongting Wen,Hulan Chen,Yu Fan,Yuzhu Tan,Zhentao Tang

To overcome the great challenge of simultaneously reducing the matrix effect and sensitively analyzing multi-mycotoxins in complex samples, a modified QuEChERS-UHPLC-MS/MS method based on novel nanomaterials was developed for the analysis of 18 mycotoxins in different matrices. The modified QuEChERS integrated traditional QuEChERS with freezing and magnetic dispersion solid phase extraction (MDSPE), which adopted an in-house fabricated nanomaterial (Fe 3 O 4 @MWCNT@Uio-67) as a purification material. To validate the sensitive and efficient analysis of the target mycotoxins, the established method was investigated on three medicinal and edible matrices. These matrices are typical representatives of complex and diverse matrices, of which the main ingredients are starch, oil, and polysaccharides, respectively. Under the optimized conditions, the linear detection range was 1.00–1250.00 μg/kg (R 2  > 0.998). The detection limits were down to 0.003–5.096 μg/kg. The accuracy (spiked recovery/66.38–139.17%) and precision (intra-RSDs/0.15–19.65%, inter-RSDs/0.23–16.40%) were both satisfactory. Compared to C 18 , the novel material presented a better ability to purify the substrate matrices, along with a more acceptable recovery. Through the comparison with other methods, the developed method was further demonstrated to be sensitive, efficient, and with great potential for the analysis of multi-mycotoxins in diverse and complex samples.

Simultaneous detection of multiple phenolic compounds in fish by gas chromatography-mass spectrometry following a modified QuEChERS cleanup

Jiali Xing,Yang Li,Ruihang Zheng,Hao Shen,Xiaorong Xu,Lingyan Mao,Xiaohu Luo,Jian Shen,Weirong Yao

Development of a modified quick, easy, cheap, effective, rugged, and safe method based on melamine sponge for multi-residue analysis of veterinary drugs in milks by ultra-performance liquid chromatography tandem mass spectrometry

Baocheng Ji,Wenhao Zhao,Xu Xu,Yu Han,Mingsha Jie,Gaigai Xu,Yanhong Bai

The purpose of this study was to develop a modified QuEChERS method based on melamine sponge for rapid determination of multi-class veterinary drugs in milks by UPLC-MS/MS. Through simple infiltration and extrusion, fast and convenient matrix purification could be achieved within several seconds, and there was no need of extra phase separation operations. Good linearity with correlation coefficient (R 2 ) ≥0.999 was obtained for all drugs in the range of 2~500 µg·kg −1 . The obtained matrix effects were within ±20% for all monitored drugs. The recoveries of all monitored drugs ranged from 60.7% to 116.0% at three spiked levels (50, 100, and 200 µg·kg −1 ), with relative standard deviations less than 7.4%. Comparatively low LODs and LOQs were obtained in the ranges of 0.1~3.8 µg·kg −1 and 0.2~6.3 µg·kg −1 , respectively. Compared with conventional purification adsorbents, melamine sponge yielded an equal or higher purification performance with matrix removal rate as high as 52.5% and acceptable recoveries in range of 60%-120% for all monitored drugs. The satisfactory results have demonstrated the good potential of melamine sponge in matrix purification for rapid determination of multiclass residues in food safety.

A magnetic hyperbranched polyamide amine-based quick, easy, cheap, effective, rugged and safe method for the detection of organophosphorus pesticide residues

Jun Wang,Zhao-Li Mou,Hui-Ling Duan,Shi-Yao Ma,Jing Zhang,Zhi-Qi Zhang

Magnetic hyperbranched polyamide amine (MHPA) was successfully prepared and applied as a QuEChERS adsorbent to the gas chromatograph-mass spectrometer (GC–MS) detection of organophosphorus pesticides (OPPs) in orange juice. Abundant in amino types and the structure of hyperbranched organic chains make MHPA to possess the clean-up function integrating classic clean-up agent primary secondary amine (PSA) with C 18 modified silica, and the magnetic property makes the operation easier and more time-saving. Compared the performance with classical clean-up agents of PSA and C 18 , better results were obtained with MHPA as adsorbent for the detection of 11 OPPs. Recoveries ranged from 75.2 to 116.2% with the relative standard deviation (RSD) of 4.1–18.9% and the limit of detection (LOD) of 0.74–8.16 ng/g. Results showed that using MHPA as adsorbent for QuEChERS sample preparation is an effective alternative with simplicity and rapidity.

Response surface–optimized QuEChERS-UPLC-MS/MS method for multi-antibiotic determination and dietary risk assessment in animal-derived foods

Rong Bao,Rongting Zhuo,Zhuxiang Zhong,Yan Yang

Antibiotic residues in animal-derived foods raise food safety concerns. This study developed a QuEChERS–UPLC–MS/MS method for the simultaneous detection of multiple antibiotics in animal-derived foods. Key QuEChERS pretreatment parameters were systematically optimized using response surface methodology with a central composite design to identify the optimal extraction solvents, salting-out agents, and clean-up sorbents. Method validation met the requirements of European Commission Implementing Regulation (EU) 2021/808, confirming suitability for rapid determination of 85 antibiotics across diverse food matrices. Analysis of 590 samples detected antibiotic residues in 39.8% of samples, representing 36 different antibiotics. Health risk assessment showed a Hazard Index (HI) < 1, indicating low risk at current consumption levels for the local population. Nevertheless, this high detection frequency highlights the need for continued monitoring of antibiotic residues in animal-derived foods.

Evaluation of Dissipation Behavior, Residues, and Dietary Risk Assessment of Fludioxonil in Cherry via QuEChERS Using HPLC-MS/MS Technique

Shunyu Yao,Zixi Zhao,Wang Lu,Xin Dong,Jiye Hu,Xiaolu Liu

The chemical fungicide fludioxonil is widely used to control post-harvest fungal disease in cherries. This study was implemented to investigate the dissipation behaviours and residues of fludioxonil on cherries. A reliable and efficient analytical method was established. Cherry samples from four product areas were analyzed by QuEChERS and HPLC-MS/MS methods with acceptable linearity (R2> 0.99), accuracy (recoveries of 81–94%), and precision (relative standard deviation of 2.5–11.9%). The limits of quantification (LOQs) and limits of detection (LODs) of cherries were 0.01 mg/kg and 0.005 mg/kg. The dissipation of fludioxonil on cherries followed first order kinetics with half-lives of 33.7–44.7 days. The terminal residues of fludioxonil were all lower than 5.00 mg/kg, which is the MRL recommended by the European Commission. According to Chinese dietary patterns and terminal residue distributions, the risk quotient (RQs) of fludioxonil was 0.61%, revealing that the evaluated cherries exhibited an acceptably low dietary risk to consumers.Keywords:fludioxonil;cherry;HPLC-MS/MS;dissipation behaviour;residues;dietary risk assessment

Synthesis of a novel β-cyclodextrin chiral stationary phase and its application to the evaluation of the enantioselective bioaccumulation and elimination behavior of tebuconazole in Rana nigromaculata tadpoles

Linbin Zheng,Meng Li,Zhouyu Jiang,Junyan Fan,Zengbo Fang,Jihuai Zheng,Yan Cui

Background The increased production and use of chiral pesticides will enhance their exposure in the environment. Chiral pesticides typically exhibit varied biological effects among these enantiomers. Therefore, it is very essential to develop and validate chiral analytical methods to investigate their potential ecological risks from a stereoselective perspective. Current separation of pesticides enantiomers relies extensively on chiral stationary phases (CSPs), while the development of β-Cyclodextrin derivatives CSPs become the research focus due to their great modifiability and excellent chiral recognition capabilities. Results A novel chiral stationary phase, 3,5-dichlorophenylaminomethyl-6-phenylenediamine-β-cyclodextrin chemically bonded silica gel (MPDCDA), was successfully prepared. Based on that, a stereoselective HPLC-MS/MS method was developed and validated for the determination of tebuconazole enantiomers in Rana nigromaculata tadpoles. After extraction by QuEChERS, the tebuconazole enantiomers were completely separated with the resolutions of 1.63 using the mobile phase of methanol-water (70/30, v/v). Good linearity (r > 0.9990) for both enantiomers over a concentration range of 0.20–500.0 ng/mL was obtained with the accuracy ranged from 6.7 % to 9.3 % and the intra-day and inter-day precisions below 6.2 % at three quality control levels. The proposed method was successfully applied in evaluating the enantioselective bioaccumulation and elimination profiles of tebuconazole in tadpoles. At the tested conditions, there was no significantly enantioselective difference in the bioaccumulation process for S - tebuconazole and R -tebuconazole. However, the elimination process of tebuconazole enantiomers was enantioselective with R -tebuconazole preferentially degraded. Significance This work provided an accurate risk assessment of chiral pesticides to non-target aquatic organisms from a stereoselective perspective. These findings would deepen our understanding of the potential ecological risks of chiral pesticides on aquatic organisms and provide scientific support for the protection of aquatic organisms and their ecological environments, as well as sustainable development.

Acid-treated ZIF-67-derived porous carbon based QuEChERS coupled with LC-MS/MS for sensitive determination of multi-pesticide residues

Mantang Chen,Libin Wan,Shuhan Yu,Li Chen,Jingjing Yu,Xiaoyu Wang,Cong Nie,Fuwei Xie,Wenfen Zhang

Simple and convenient synthesis of a purification material of CZIFA. • Enhanced purification performance of CZIFA by acid treatment strategy. • Analysis and detection of pesticide residues in complex matrices. • Expanded application of ZIF-derived carbon materials in food safety detection. Porous carbon-based QuEChERS purification material (CZIFA) was synthesized through a straightforward calcination and acid treatment process using Zeolitic Imidazolate Framework-67 (ZIF-67) as the precursor. The abundant adsorption sites and excellent clean-up capability of CZIFA resulting from acid treatment were confirmed through a series of characterization and performance evaluations. Combined with LC-MS/MS, a modified QuEChERS method using CZIFA as the adsorbent was developed for the simultaneous detection of 48 pesticide residues in tobacco. Under optimized conditions, the established method achieved low limits of detection (0.02–9.92 μg/kg), wide linear ranges (2–200 μg/L), and satisfactory precision. The average recoveries of the method were in the range of 80.1–119.7% with the relative standard deviations (RSDs) of <9.5%. This study provides a novel and efficient functionalized material for analyzing pesticide residues in complex matrices. Especially, it expands the application of ZIF-derived carbon materials in food safety detection. Download: Download high-res image (298KB) Download: Download full-size image