MOLECULES
·
2022
·Vol. 27
·期 4
·1318
·
IF 4.927
Jia Zheng,Zhanglan He,Kangzhuo Yang,Zhipeng Liu,Dong Zhao,Michael C. Qian
Wuliangye baijiu is one of the most famous Chinese liquors with a protected geographical indication. This study used LiChrolut®EN-based solid-phase extraction (SPE) and fractionation combined with comprehensive two-dimensional chromatography-time-of-flight mass spectrometry (GC×GC-TOFMS) to unveil its volatile composition. The volatiles were isolated with LiChrolut®EN-based SPE and traditional liquid-liquid extraction (LLE). The neutral/basic fractions from LLE and the SPE were fractionated on a LiChrolut®EN SPE column and analyzed by comprehensive GC×GC-TOFMS. Compared with LLE, more esters and alcohols were detected in the SPE-based extraction. The SPE fractionation and GC×GC-TOFMS analysis resulted in the identification of about 500 volatile compounds in more than 3000 peaks of the Wuliangye baijiu. The approach simplifies the complex baijiu composition into functional group-based fractions for reliable identification and analysis. This study provided a confidence volatile identification approach for Chinese baijiu based on the SPE fractionation GC×GC-TOFMS.Keywords:baijiu;volatile fractionation;Wuliangye;LiChrolut®EN SPE;GC×GC-TOFMS
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2019
·
IF 3.206
Wen Nie,Fangfang Wang,Runqing Hao,Lu Zhang,Qian Chen,Fanmei Wei,Xiaotong Li,Robert Loffredo,Zhenbo Liu,Yongming Liu
For aqueous two-phase extraction (ATPE), adsorbents such as primary secondary amine (PSA) are usually used to remove fat and protein in meat samples. However, it was determined that PSA adsorbed approximately 5% of measured sulfonamides (SAs), which is the reason for the low recovery rate. To overcome this adverse PSA effect, a solid phase extraction (SPE) method was used for purification and enrichment after the formation of aqueous two-phase. Based on these, A new aqueous two-phase sample pretreatment method with solid phase extraction (ATP-SPE) to detect sulfonamides in fish meat is proposed. Fluorescence quenching showed that for 6 SAs, hydrogen bonding and van der Waals force played the major role in the binding reaction with fish serum albumin protein. In addition, in the 80% ACN aqueous solution, a slow protein denaturation took place and the drugs bound with the protein were released, which is more conducive to the aqueous two-phase extraction. In order to obtain better separation effect, the factors for synthesis of hydrophobic-lyophobic balance (HLB) packing for SPE were explored. Stirring speed is the most important factor affecting the particle size of microspheres . After purification and enrichment by SPE, samples were directly analyzed by HPLC. The analytical process was validated in the fish sample matrix by the analysis of spiked blank samples. The mean recoveries of this method were 80.1–95.1% with RSD values of 1.37–3.95%. The detection limits were 5.8–11.7 ng/g. The new ATP-SPE pretreatment method provides a new way for better recovery of veterinary drugs in meat products.
研究领域:
分析化学
·
食品科学
·
药理学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2013
·Vol. 52
·期 8
·932-937
·
IF 0.794
Liu Xiaofang,Zhou Shu,Zhu Quanfei,Ye Yong,Chen Huaixia
A sample pretreatment method, solid-phase extraction combined with dispersive liquid–liquid microextraction (SPE–DLLME), was established for the sensitive determination of polycyclic aromatic hydrocarbons (PAHs) in smoked bacon samples. In the SPE–DLLME process, three PAHs including naphthalene (Naph), phenanthrene (Phen) and pyrene (Pyr) were extracted from samples and transferred into C18 SPE cartridge. The target analytes were subsequently eluted with 1.2 ml of acetonitrile–dichloromethane (5:1, v/v) mixture solution. The eluent was injected directly into the 5.0 ml ultrapure water in the subsequent DLLME procedure. The sedimented phase was concentrated under a gentle nitrogen flow to 120.0 µl. Finally, the analytes in the extraction solvent were determined by high-performance liquid chromatography with a ultra-violet detector. Some important extraction parameters affecting the performance, such as the sample solution flow rate, breakthrough volume, salt addition as well as the type and volume of the elution solvent were optimized. The developed method provided an ultra enrichment factors for PAHs ranged from 3478 to 3824. The method was applied for the selective extraction and sensitive determination of PAHs in smoked bacon samples. The limits of detection (S/N = 3) were 0.05, 0.01, 0.02 μg kg−1 for Naph, Phen, Pyr, respectively.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF SEPARATION SCIENCE
·
2013
·
IF 2.591
Yihui Chen,Tingting Wang,Junfeng Ma,Zhen Liang,Mingliang Chen,Jianghua Fang,Haoqi Gao,Lihua Zhang,Yukui Zhang
An SPE cartridge based on an ampholine-functionalized hybrid organic–inorganic silica sorbent has been adopted for the analysis of aromatic amines including 4-aminobiphenyl, benzidine, 2-naphthylamine, p -chloroaniline, 2,4,5-trimethylaniline, and 3,3′-dichlorobenzidine. Crucial variables governing the extraction efficiency of the material such as the pH of sample, sample loading volume, solvent used for elution, and elution volume have been thoroughly optimized. The adsorption capacities for the six aromatic amines ranged from 0.17 to 1.82 μg/mg. The recoveries of aromatic amines spiked in textile samples ranged from 78.9 to 103.0%, with RSDs of 1.1–11.9% ( n = 3). Moreover, the extraction efficiency of the ampholine-functionalized hybrid organic–inorganic silica sorbent was at least comparable with that of Oasis WCX.
研究领域:
分析化学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2021
·
IF 4.821
Yueting Liao,Yaohai Zhang,Qiyang Zhao,Wei Xiang,Bining Jiao,Xuesu Su
Metal organic framework MIL-101(Cr) was successfully synthesized as a selective adsorbent by a facile self-assembly technique and combined with UPLC-MS/MS for enrichment and determination of neonicotinoids in fruit juices and tea beverages. Therein, MIL-101(Cr) was characterized by Fourier transform infrared spectrometry, scanning electron microscopy, X-ray diffraction, and N 2 adsorption–desorption isotherms. Box-Behnken design was applied to optimize the significant variables including the sorbent amount, pH of the matrix, eluant volume, extraction time and desorption time. The optimized conditions were sorbent amount of 20 mg, eluent volume of 1 mL, extraction time of 5 min and desorption time of 4 min. Under the optimized conditions, excellent sensitivity was achieved with the limit of detection of 0.0019–0.02 μg/L and limit of quantification of 0.0063–0.067 μg/L. Good linearity (R 2 ≥ 0.9988) was obtained within the range of 1–1000 μg/L, and the recovery was 71.04%-101.64% with relative standard deviations (RSDs) of 1.25%-8.82% in spiked samples. The inter- and intra-day RSDs were both<8.54%. The adsorption isotherms investigated for acetamiprid, thiacloprid, and imidacloprid pesticides better fitted with the Freundich adsorption isotherm with bimolecular adsorption capacity of 71.43, 68.49, and 50.38 mg/g, respectively. These results indicate that the nanocomposite is feasible for adsorption of the target analytes at trace amounts from fruit juices and tea beverages.
研究领域:
分析化学
·
环境科学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
IONICS
·
2021
·Vol. 28
·期 2
·779-788
·
IF 2.817
Guo Zhihao,Wu Yuqi,Li Xinhai,Wu Xianwen,Hu Qiyang,Wang Zhixing,Guo Huajun,Peng Wenjie,Yan Guochun,Wang Jiexi
Employing the solid polymer electrolyte (SPE) instead of traditional liquid electrolyte is an effective way to develop high safety and high-energy density solid-state lithium batteries. Herein, for the first time, the Ni 3 B 2 O 3 (NBO) nanorods are incorporated into polyethylene oxide (PEO)-based SPE. Particularly, the optimized NBO-embedded SPE shows a high ionic conductivity of 8.5 × 10 −5 S cm −1 at 30 °C, lowering the operating temperature of PEO-based SPE substantially. The corresponding LiFePO 4 /Li battery demonstrates a high discharge capacity of 154 mAh g −1 after 80 cycles at 0.2 C under 30 °C, with favorable capacity retention of 97.5%. The remarkable properties are attributed to the high ionic conductivity of modified SPE at ambient temperature, which is resulted from the decreased crystallinity and melting transition point, increased movement of PEO chain, and promotion of lithium salt dissociation, as well as the formation of the lithium ion migrating pathway on the interface between PEO and NBO nanorods.
研究领域:
材料科学
·
电化学
·
能源存储
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2026
·
IF 2.8
Haiyang Cui,Dongliang Yang,Yonggang Zheng,Jing Li,Hairui Yan,Xiaoli Gao
Steroids and their metabolites play crucial roles in reproductive health, endocrine diseases, and tumor development. Comprehensive analysis of these compounds is essential for both mechanistic investigations and clinical evaluations. Although comprehensive analytical methods have been established for steroids in human clinical samples, their direct application to rat specimens remains limited, particularly with the absence of validated methods for detecting certain hydroxylated steroid metabolites in vivo. This study developed highly sensitive solid-phase extraction coupled with ultra-high-performance liquid chromatography-tandem mass spectrometry methods for the quantitative analysis of 29 steroid metabolites. Through optimized derivatization of steroids and integration of two-dimensional liquid chromatography techniques, the method effectively reduces interference from non-volatile salts and overcomes trace-level detection challenges. Method validation demonstrated a wide linear range (0.002–250 ng/mL), low limits of quantification (2–100 pg/mL), high accuracy (88–114%), and precision (intra- and inter-batch CV ≤14%). The method exhibited acceptable extraction recovery, matrix effects, and stability, confirming compliance with regulatory standards. The validated method was successfully applied to characterize serum steroid metabolic profiles in both N -methyl-N-nitrosourea-induced breast cancer and ovariectomized rat models, revealing alterations in estrogen 2-hydroxylation and pregnenolone 21-hydroxylation pathways mediated by key steroidogenic enzymes, including CYP1A1/CYP1B1 and potentially CYP21A2-independent mechanisms, providing robust support for preclinical research on steroid-related diseases.
✓ 已验证
产品关联
DOI
PubMed
高影响因子
SEPARATION AND PURIFICATION TECHNOLOGY
·
2025
·
IF 9
Yan Gao,Kangjia Sheng,Jiao Long,Junjie Yao,Tao Bao,Sicen Wang
Sample pretreatment prior to analysis is crucial for enhancing the quality of detection of target analytes. Herein, we propose a novel, easy-to-assemble continuous gas lift extraction device for the extraction of pharmaceutical pollutants. As a proof-of-concept, we assess the performance of the developed system through laboratory-scale experiments utilizing a homemade adsorbent. This device works by inserting an upright hollow cylindrical tube into the sample solution, with the upper end fitted with an air inlet and the lower end is equipped with a porous adsorbent. When gas is injected into the tube, the sample solution is circulated through the porous adsorbent driven by the pressure differential created by gas movement, thereby facilitating capture of target components within the sample solution. The adsorbent can be replaced based on the target molecule. We synthesize a type of porous adsorbent in the shape of a round cake, made from quartz sand that is surface-modified with a Zr-based metal–organic framework, using a solvothermal method. The experimental results indicate that the developed extraction method exhibits good performance with the limit of detections of 0.045–0.25 ng/mL, thereby demonstrating its potential for real-world applications.
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
Heliyon
·
2024
·
IF 3.4
Shunqin Chen,Han Yang,Shan Zhang,Faze Zhu,Shan Liu,Huan Gao,Qing Diao,Wenbo Ding,Yuemeng Chen,Peng Luo,Yubo Liu
This study developed an online solid-phase extraction ultra-high performance liquid chromatography-tandem mass spectrometry (Online-SPE-UHPLC-MS/MS) method for the analysis of 28 illegal drugs in sewage. To achieve this, 28 isotope internal standards (ISTDs) were added to 3 mL sewage samples, the pH was adjusted to 7–8 using hydrochloric acid or 20% ammonia water, followed by centrifugation, filtration, and analysis using UHPLC-MS/MS. The results indicated an excellent linearity of 1–300 ng L −1 , and cotinine in the concentration range of 20–6000 ng L −1 , linear correlation coefficient R 2 > 0.995, with the limit of detection (LOD) of 0.01–6 ng L −1 , and a limit of quantification (LOQ) of 0.1–20 ng L −1 . The addition of three concentrates of low (2 ng L −1 /40 ng L −1 ), medium (20 ng L −1 /400 ng L −1 ), and high concentration (200 ng L −1 /4000 ng L −1 ) demonstrated the matrix effect of the target compound between ± 22.0%. The extraction recovery was 70.0–119.4%, and a percent accuracy of 75.7–118.1%. Similarly, the intra- and inter-day precisions were 1.8–20.0% and 1.5–18.9%, respectively. The results cemented the sensitivity, accuracy, reliability, strong specificity, and reproducibility, which can be used to screen 28 illegal drugs in sewage for trace analysis.
研究领域:
环境科学
·
分析化学
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Analytical Methods
·
2021
·Vol. 13
·期 39
·4691-4698
·
IF 2.896
Long Li,Kehan Xu,Zuohua Huang,Xinxin Xu,Jibran Iqbal,Liang Zhao,Yiping Du
A new in-syringe membrane SPE and solid-phase visible spectral method was proposed for the rapid extraction and visible spectral determination of trace Cu2+. The chelation and membrane SPE can be accomplished in a syringe. The yellow Cu(DDTC)2 complex was separated using a polyethersulfone membrane from the sample solution. Then, the complex can be detected directly on the polyethersulfone membrane utilizing solid-phase visible absorbance spectra without elution. The proposed method simplified the experimental procedure and improved the sensitivity to the μg L−1 level. Furthermore, this method is environmentally friendly since it avoids the use of organic solvents. After the investigation of the influence of different variables on the membrane SPE procedure, water and blood plasma were analyzed to validate the proposed method. A LOD of 0.04 μg L−1 and recoveries of 96.0–103.7% confirmed that the present work can be applied for the determination of trace Cu2+ in water and blood plasma samples.
研究领域:
分析化学
·
环境科学
·
光谱学
✓ 已验证
DOI
PubMed
高影响因子
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
·
2018
·Vol. 411
·期 2
·507-515
·
IF 3.307
Yang Yi,Yin Shuo,Yang Danni,Jiang Yang,Li Yongxin,Zhou Chen,Sun Chengjun
A novel carboxyl Fe 3 O 4 magnetic nanoparticle-based solid-phase extraction combined with high-performance liquid chromatography was developed for the analysis of oxytetracycline, tetracycline, demeclocycline, metacycline, chlortetracycline, and doxycycline in water samples. Driven by the electrostatic interaction and the strong chelation between tetracyclines and iron ions, tetracyclines in samples were adsorbed onto the adsorbents. The adsorbed analytes were subsequently eluted with oxalic acid and separated with a C 18 column under gradient condition with a mobile phase consisting of methanol, acetonitrile, and oxalic acid at a flow rate of 0.5 mL/min. The detection was performed at variable ultraviolet wavelengths. Under optimized conditions, the developed method gave an enrichment factor of 33.3, linearity ranges of 5.00–1000 μg/L, detection limits of (2.86–5.19) × 10 -2 μg/L, quantification limits of (9.54–17.3) × 10 -2 μg/L, recoveries of 76.2–98.0%, and intra- and inter-day RSDs of 0.132–15.5% and 2.28–14.5% for these tetracyclines. The established method was successfully applied for the determination of these six tetracyclines in tap water, river water, pond water, and lake water samples.
ᅟ
研究领域:
环境科学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MOLECULES
·
2020
·Vol. 25
·期 4
·839
·
IF 3.267
Yueqing Xu,Liangxiao Zhang,Ruinan Yang,Xu Yu,Li Yu,Fei Ma,Hui Li,Xiupin Wang,Peiwu Li
Vitamin K1is one of the important hydrophobic vitamins in fat-containing foods. Traditionally, lipase is employed in the determination of vitamin K1to remove the lipids, which makes the detection complex, time-consuming, and insensitive. In this study, the determination of vitamin K1in fat-containing foods was developed based on ultrasound-assisted extraction (UAE), solid-phase extraction (SPE) combined with liquid chromatography–tandem mass spectrometry (LC-MS/MS). The optimal conditions for extraction of vitamin K1were material–liquid ratio of 1:70 (g/mL), extraction temperature of 50 °C, extraction power of 700 W, extraction time of 50 min, material-wash fluid ratio of 1:60 (g/mL), and 8 mL of hexane/anhydrous ether (97:3,v/v) as the elution solvent. Then, vitamin K1was analyzed on a ZORBAX SB-C18 column (50 mm × 2.1 mm, 1.8 μm) by gradient elution with water (0.01% formic acid) and methanol (0.01 formic acid + 2.5 mmol/L ammonium formate) as the mobile phase. The limit of detection (LOD) and limit of quantification (LOQ) were 0.05 and 0.16 μg/kg, respectively. Calibration curve was linear over the range of 10–500 ng/mL (R2> 0.9988). The recoveries at three spiked levels were between 80.9% and 119.1%. The validation and application indicated that the proposed method was simple and sensitive in determination of vitamin K1in fat-containing foods.Keywords:ultrasound-assisted extraction;solid-phase extraction;LC-MS/MS;vitamin K1;foods
研究领域:
分析化学
·
营养学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
危险品化学品经营许可证（带存储）