Food Analytical Methods
·
2022
·Vol. 15
·期 9
·2479-2486
·
IF 3.498
Zhang Shengnan,Li Zhibo,Qi Yanxia,Yu Pei,Zhao Qiancheng
The determination of 2-acetyl-1-pyrroline (2-AP), which is an important flavour compound of crustaceans and has a low odour threshold of 0.05 μg/L in water, is still a challenge due to the instability and trace levels of 2-AP in food samples. In this study, 2-AP was trapped by o-phenylenediamine and subsequently purified by the dispersive solid-phase extraction and dispersive liquid–liquid microextraction (DSPE-DLLME) methods for HPLC–UV analysis. The developed method was simple, fast and sensitive for the determination of 2-AP in shrimp. Under the optimized DSPE-DLLME conditions, the developed method exhibited excellent linearity ( R 2 = 0.996) and a low limit of detection (LOD, 1.77 μg/kg) and limit of quantitation (LOQ, 5.33 μg/kg). The recoveries of 2-AP in shrimp ranged from 86.3 to 101.6%. In addition, the developed method was applied to detect 2-AP levels in baked shrimp (ranging from 5.6 to 12.6 μg/kg), indicating that the formation of 2-AP could be observed in thermally treated shrimp depending on heating temperature and time. In summary, the developed method has potential application for the trace determination of 2-AP in shrimp due to its convenience and high sensitivity.
研究领域:
食品科学
·
分析化学
✓ 已验证
DOI
高影响因子
MOLECULES
·
2024
·Vol. 29
·期 3
·567
·
IF 4.2
Yayun Guo,Zhe Wang,Yi He,Huanhuan Gao,Hongmei Shi
Aspergillus carbonariusis known to produce the carcinogenic ochratoxin A (OTA) in grapes. The metabolism process before OTA biosynthesis influences the content and composition of the volatile compounds in grapes. In this study, a self-established method based on QuEChERS coupled with high-performance liquid chromatography–fluorescence detection (HPLC-FLD) was used to determine the OTA levels during a seven-day contamination period. The results showed that OTA was detected on the second day after contamination withA. carbonarius. Thus, the first day was considered as the critical sampling timepoint for analyzing the volatiles in grapes before OTA biosynthesis. Additionally, the volatile compounds in grapes were analyzed using headspace solid-phase microextraction gas chromatography–mass spectrometry (HS-SPME-GC-MS) and dispersive liquid–liquid microextraction gas chromatography–mass spectrometry (DLLME-GC-MS). The corresponding data were evaluated via multivariate data analysis using projection methods, including PCA and OPLS-DA. The results indicated significant differences in the nine volatile compounds in grapes contaminated withA. carbonariusbefore OTA biosynthesis. The results of the Pearson correlation analysis showed positive correlations between ethyl acetate, styrene, 1-hexanol and OTA; (E)-2-hexenal and nerolic acid were negatively correlated with OTA. Overall, these findings provide a theoretical basis for the early prediction of OTA formation in grape and grape products using GC-MS technology.Keywords:volatile compounds;Ochratoxin A;QuEChERS-HPLC-FLD;HS-SPME-GC-MS;DLLME-GC-MS;OPLS-DA
研究领域:
食品科学
·
真菌学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
FOOD CHEMISTRY
·
2020
·
IF 6.306
Lingfei Ma,Yanfei Wang,Haipu Li,Fangyuan Peng,Bo Qiu,Zhaoguang Yang
Monitoring neonicotinoid residues in grains is of significant interest for the proper assessment of pesticide exposure to human. The quick, easy, cheap, effective, rugged, and safe extraction method combined with dispersive liquid-liquid micro-extraction (QuEChERS-DLLME) was developed for extracting, purifying, and concentrating seven common neonicotinoid pesticides from the grains (rice, millet, and maize). Water and acetonitrile were used in tandem as extractants in QuEChERS, while water, acetonitrile, and trichloromethane in DLLME acted as the external phase, dispersant, and extractant, respectively. Comprehensive consideration of the single factor test and response surface method to optimize parameters including type and volume of extractants and dispersant. The evaluation showed that the QuEChERS-DLLME method held excellent linearity ( R 2 > 0.99). The limits of quantitation ranged from 0.003 to 0.08 µg kg −1 for the seven insecticides. The recoveries were in the range of 62–118%, and good reproducibility was obtained with a relative standard deviation below 15%.
研究领域:
农业化学
·
分析化学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Separations
·
2022
·Vol. 10
·期 1
·1
·
IF 3.344
Xian Zhang,Luyun Zhang,Dan Zheng,Zhenzhen Xia,Maomin Peng,Danling Sun,Xizhou Hu,Xitian Peng
In the current study, an effective and simple procedure of extraction for the four benzophenone compounds from water samples was achieved by dispersive liquid–liquid microextraction (DLLME) based on the solidification of floating organic droplets (SFO) with a natural monoterpene enol as the extractant. As a natural, high solidification point, inexpensive, and environmentally friendly hydrophobic solvent, α−terpineol was selected firstly as an extractant for DLLME and could be collected and transferred easily after extraction by solidification at a lower temperature. Several main parameters closely related to extraction efficiencies, such as volume of extractant, extraction time, pH and salt concentration of the sample solution, temperature, and time of the solidification process, were investigated in detail. The results showed that the established method had good extraction performance for benzophenone compounds with enrichment factors in the range of 29–47. Furthermore, the linearities were over the range of 2–2000 µg/L, and the limits of detection were 0.12–0.53 µg/L for four benzophenone compounds. The recoveries ranged from 80.2% to 108.4%, with RSDs (intra- and inter-assay) less than 8.5%. At last, the method applicability was investigated by the determination of the benzophenone compounds in aqueous solutions, and satisfactory recoveries (83.0–107.0%) were acquired. Taken together, α−terpineol, a natural monoterpene enol, was first used as an extractant of DLLME-SFO, which provided an alternative method with simplicity and rapidity for the determination of benzophenone compounds in aqueous samples.Keywords:α−terpineol;dispersive liquid–liquid microextraction (DLLME);solidification of floating organic droplet (SFO);benzophenone compounds
研究领域:
分析化学
·
环境科学
✓ 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 PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2019
·
IF 2.983
Qianqian Cai,Tianyu Zhao,Lianjun Zhang,Pan Zhao,Yajie Zhu,Haiyan Xu,Xiaohong Hou
Dispersive micro-solid-phase extraction (DMSPE) combined with dispersive liquid–liquid microextraction based on the solidification of a floating organic droplet (DLLME-SFO) was successfully developed for extraction and depuration of pantoprazole in rat plasma. The remarkable metal organic framework (MOF), MIL-101(Cr) was used as DMSPE adsorbent. The detection of pantoprazole was performed by convenient HPLC-UV. In the extraction of pantoprazole from plasma samples, small molecule compounds, including the target and abundant impurities, were easily admitted into the porous structure of MIL-101 (Cr) material in DMSPE; while, macromolecular compounds were handily excluded from the adsorbent. Next, the depuration process was achieved by removal of small polar impurities in DLLME-SFO. Influential factors were systematically optimized for ideal enrichment and depuration efficiency. Under the optimal conditions, a satisfactory linearity range from the lower limit of quantification (LLOQ, 100 ng/L) to 10 000 ng/L with the correlation coefficients ( r ) of 0.9934 was obtained. The LLOQ was 100 ng/mL and the relative recoveries were ≧ 73.2 ± 4.8%. The approving reproducibility, acceptable accuracy, and stability were all within the acceptance limits. This proposed method presented the advantages of environment-friendly, low-cost, recyclable, low impurity, and preferable applicability. It could offer a new idea for the pretreatment and pharmacokinetic study of pantoprazole in rat plasma.
研究领域:
分析化学
·
药物代谢动力学
·
医学检验
✓ 已验证
产品关联
DOI
PubMed
高影响因子
RSC Advances
·
2025
·Vol. 15
·期 21
·16734-16741
·
IF 4.6
Xiaofang Sun,Chuanbin Zhang,Youwen Pan,Haiyang Mei,Jiawen Song,Mengfei Zhou
The traditional standard method for the determination of the heavy metal pollutant antimony (Sb) in water, 5-Br-PADAP spectrophotometry, involves the consumption of many kinds of chemical reagents and has low sensitivity. For highly toxic liquid and gas containing Sb(III), this paper presents a green determination method based on UV/O3 synergistic oxidation-malachite green-dispersive liquid–liquid microextraction (DLLME)-spectrophotometry, which can achieve the enrichment of a trace amount of antimony in water and high-precision detection. Using the selective complexation and color development of protonated alkaline dye and the solubility difference of the complexes involved, an enrichment and determination method for trace Sb(V) in surface water was established for the first time. Based on the feature of the UV/O3 system of rapid and complete oxidation of Sb(III), and the easy elimination of the disturbance of residual oxidant, the green determination method for trace total antimony (TSb) was constructed based on advanced oxidation processes (AOPs). To verify the validity of the proposed method, all the process parameters and environmental factors affecting the oxidation efficiency of Sb(III) and the enrichment performance of DLLME were investigated and optimized. The results showed that the proposed method exhibited good linearity (R2 = 0.9943), a low method detection limit (MDL = 0.3208 μg L−1), and high precision (1.63%) and accuracy (0.64%) in the range of 1–30 μg L−1, under the optimized process conditions. By the difference method, the trace free antimony (Sb(III), Sb(V)) and total antimony (TSb) can be determined simultaneously.
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
Journal of Food Measurement and Characterization
·
2026
·
IF 3.3
Yang Fan,Ruan Ya,Yang Yaling
For the first time, copper-doped amino acid carbon dots (Cu/Asp-CDs) are reported as a green peroxidase-like nanozyme. Using Cu 2+ as the metal dopant and L-aspartic acid (Asp) as the ligand, Cu/Asp-CDs exhibit high catalytic activity and stability. They efficiently catalyze the oxidation of butylated hydroxyanisole (BHA) in the presence of 4-aminoantipyrine (4-AP) and H 2 O 2 , producing a visible color change for rapid and specific BHA detection. Based on this, a portable, cost-effective colorimetric sensor was developed, showing high sensitivity, selectivity, and linearity from 0.67 to 66.67 μM, with a detection limit of 0.27 μM. To extract BHA from edible oils, a deep eutectic solvent of choline chloride and thymol (1:2 molar ratio) was used in liquid–liquid microextraction, achieving recoveries of 89.0–109.0%. Combined with the nanozyme, this method enables a practical, rapid (within 20 min) assessment of synthetic antioxidants, offering a reliable tool for food quality monitoring.
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
2026
·
IF 5.1
Qing-nan Chen,Yun-e Bai,Yao Ma,Rui Liao,Lu-lu Wang,Shuang Hu,Jian- ping Gao
Latex-bearing plants have gained global attention, but few studies have been reported on Codonopsis pilosula (Franch.) Nannf.( C. pilosula ) latex. In this research, we established a UHPLC-MS/MS method to investigate the constituents in C. pilosula latex. Analysis revealed that the latex of C. pilosula contains alkaloids, terpenoids, and fatty acids, with fatty acids being one of the primary metabolites distinguishing the latex from above-ground (DS) and below-ground (DX) parts of C. pilosula. To evaluate the quality of C. pilosula latex, an approach of dispersive liquid-liquid microextraction with solidification of the floating organic drop (DLLME-SFO) methodology was developed to quantitatively analyze the contents of three fatty acids (palmitic, linoleic, and stearic) in the latex of C. pilosula . The ideal extraction conditions involve injecting 20 μL of dodecanol extractant into a 5 mL 10% NaCl solution at pH 3.0, followed by 20 min at 700 rpm. The three components mentioned above have enrichment coefficients ranging from 48 to 50. The quantification limits were between 0.23 and 0.25 μg/mL, and three components demonstrated good linearity in their respective linear ranges (R 2 > 0.995). The satisfied precision and recovery rates were 1.26 to 8.05% and 92.38 to 101.53%, respectively. By quantitatively analyzing the three fatty acid contents in the latex of C. pilosula , the results showed that palmitic and linoleic acids were able to successfully distinguish the latex of C. pilosula from different parts, which laid the foundation for the quality evaluation of C. pilosula , and provided a reference for the utilization of C. pilosula , a medicinal food source.
✓ 已验证
产品关联
DOI
高影响因子
INSTRUMENTATION SCIENCE & TECHNOLOGY
·
2021
·
IF 1.584
Zhao-chan Liu,Li Yang,Rong-rong Xing,Xuan Chen,Xiao-hong Bai,Shuang Hu
This work describes three phase dispersive liquid-liquid microextraction based on reverse micelles for the determination of Q-markers of cinnamic acids (caffeic acid, p-hydroxycinnamic acid, ferulic acid, and cinnamic acid) in traditional Chinese medicine followed by high performance liquid chromatography (HPLC) analysis. The variables influencing the procedure were optimized separately. Enrichment factors from 110 to 189, linearities from 1.2 to 960 ng mL−1 with r2 exceeding 0.9943, detection limits from 0.1 to 0.6 ng mL−1, excellent precision with relative standard deviations below 5.6%, and good relative recoveries from 80.0% to 113.3% were achieved. In addition, the mechanism of the procedure was explored by comparison with conventional dispersive liquid-liquid microextraction at the optimum conditions. The results showed that the developed microextraction procedure improved the sensitivity and consumed less organic solvent and is a greener approach.
研究领域:
分析化学
·
中药学
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICAL LETTERS
·
2022
·
IF 2.267
Hui Cao,Zixin Chen,Yanan Kong,Ziqi Wei,Tai Ye,Min Yuan,Jinsong Yu,Xiuxiu Wu,Liling Hao,Fengqin Yin,Fei Xu
Rapid dispersive liquid-liquid microextraction (DLLME) based on the solidification of a switchable hydrophilicity solvent (SHS) was established for the preconcentration of pyrethroid pesticides from grain prior to determination using high‐performance liquid chromatography (HPLC) with photodiode array (PDA). Lauric acid was selected to be the switchable hydrophilicity solvent due to its conversion between hydrophobic and hydrophilic forms and solidification at low temperature, thereby avoiding a time-consuming centrifugation step. The results show that the optimal conditions for pyrethroid pesticides included 30 mmol/L lauric acid, hydrochloric acid as the hydrogen donor, a 1:1.8 stoichiometric ratio of sodium laurate and hydrochloric acid, an extraction temperature of 50 °C, an extraction time of 8 min, and a solidification time of 3 min. Under the optimal conditions, this approach provided a high enrichment factor (308.4 to 330.2), a short pretreatment period of less than 15 min, and sensitive detection limits from 5 to 20 ng/g suitable for the analysis of food. The method was employed for the determination of pyrethroid pesticides in grain. The recoveries were 84.3% to 115.7%, and the relative standard deviation was less than 9.9%.
研究领域:
分析化学
·
食品安全
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Chunjian Wu,Li Wang,He Li,Shujuan Yu
The presence of potential carcinogen 4(5)-Methylimidazole (4-MeI) in foods causes much concern, stressing the need of a sensitive determination means. Here, we proposed a high-sensitivity method to determine 4-MeI in biscuits using dansyl chloride derivatization and disperse liquid-liquid micro-extraction (DLLME) followed by a liquid chromatography-ion trap mass spectrometry (LC-IT-MS) analysis. This developed method was subsequently compared to the solid phase extraction combining with liquid chromatography-triple quadrupole mass spectrometry (SPE-LC-QqQ-MS) method. The optimized derivatization conditions were 30 °C and 10 min. Results suggested that the column retention time (RT) was significantly extended, and the MS signal response of 4-MeI-dansyl derivative was also amplified. The developed DLLME-LC-IT-MS method in 4-MeI determination provided satisfactory linearity in a range of 0.5–300 ng/mL (R 2 > 0.9991), inter-day accuracy (87-102%) and precision (%RSD ≤ 13.6%) with the quantification limit of 0.2 ng/mL, which obtained similar results comparing to the conventional SPE-LC-QqQ-MS method.
研究领域:
分析化学
·
食品科学
·
质谱分析
✓ 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）