Toxicologie Analytique et Clinique
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2025
·
IF 1.7
Jiajun Sun,Xiaolong Zhang,Mengchao Wang,Xiaoyu Zhou,Yuxuan Chen,Jinlei liu,Yinyin Dai,Kundi Zhao,Yaqin Sun,Jie Gu,Huimin Zhang,Shengnan Zhang,Amin Wurita,Koutaro Hasegawa
Purpose Fluoxetine is a clinically used antidepressant, due to its slimming effect, unscrupulous elements will add it to slimming products. The aim of this study was to establish an optimized derivatization method for fluoxetine and norfluoxetine to be analized by a gas chromatography-tandem mass spectrometry (GC-MS/MS) and apply it to real case. Methods Hair samples were washed and cut into approximately 2 mm, and 50 mg was added to the internal standard and hydrolyzed with 1% sodium hydroxide solution. Add 3 mL ethyl acetate, vortex and centrifuge; urine samples were taken as 1 mL and then added to the internal standard and 3 mL ethyl acetate, then submitted to vortex and centrifugation. The supernatant was evaporated to dryness under a nitrogen gas stream and then derivatized by adding 25 μL ethyl acetate and 25 μL HFBA at 70 °C for 45 minutes and later analyzed by GC-MS/MS. The derivatisation procedure for the remaining derivatisation reagents TFAA, FPPA, MSTFA and 99% BSTFA + 1% TMCS was the same as above. Result Fluoxetine and norfluoxetine were analyzed by GC-MS/MS and the validation data were satisfactory. The derivatization reagent HFBA was the most effective for the modification of fluoxetine and norfluoxetine. The concentrations of fluoxetine in hair and urine extracts were 40.9 ng/mg and 10.8 ng/mL, respectively; the concentrations of norfluoxetine were 4.94 ng/mg and 7.57 ng/mL, respectively. Conclusion A method for the determination of fluoxetine and norfluoxetine in human hair and urine by GC-MS/MS was developed and applied to real cases. Furthermore, the chemical modification effects of five derivatization reagents on fluoxetine and norfluoxetine were compared, and the best effect was obtained by HFBA at 70 °C for 45 min.
研究领域:
分析化学
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毒理学
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临床医学
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FLAVOUR AND FRAGRANCE JOURNAL
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2025
·
IF 2
Hongyan Chen,Xingyu Miao,Xian Chen,Na Wang,Xin Fan,Qi Zhang,Wenjiang Dong,Lunzhao Yi
The Yunnan Province is the primary coffee-growing region in China. In this study, the flavour components of seven arabica coffee varieties in Yunnan were detected by headspace solid-phase microextraction-gas chromatography time-of-flight mass spectrometry (HS-SPME-GC-TOF-MS) and a total of 178 volatile components were annotated. There were 31 aroma compounds with 1 ≤ rOAV < 100 and 41 aroma compounds with rOAV ≥ 100. According to the aroma characteristics, defined by the relative odour activity value (rOAV) ≥ 1, the arabica coffee in Yunnan primarily exhibits fruit, sour, nut and floral aromas. Particularly, the isobutyl acetate and n-butyric acid found in Bourbon varieties enhance its fruit and sour aromas. In contrast, Geisha has a prominent floral aroma. Additionally, the 2,3-dimethyl-5-methylpyrazine present only in Catuai significantly contributes to its nutty aroma. The present results provide a valuable theoretical basis for understanding the aroma characteristics of different varieties of arabica coffee and their key underlying components.
研究领域:
食品科学
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分析化学
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植物代谢组学
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农产品品质
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挥发性有机化合物
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JOURNAL OF CHROMATOGRAPHY A
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2025
·
IF 4
Huanhuan Jiang,Qibin Li,Yang Yang,Jingcong Dai,Li Wang,Richard D Cannon,Xiaojing Dong,Ting-li Han,Lina Hu
Short-chain fatty acids (SCFAs) are prominent regulators of host physiology and are closely related to the pathophysiology of many metabolic diseases. SCFAs are predominately generated by microbial fermentation of dietary fiber in the gut. Therefore, efficient, reproducible, and affordable analytical methods are needed to identify and quantify SCFAs in a complex fecal sample. In this study, five different SCFAs (acetic acid, butyric acid, propionic acid, valeric acid, and isobutyric acid) were compared using six different extraction methods (HCl-DE, NaOH-Hexane, H 3 PO 4 -Butanol, H 3 PO 4 -EA, NaHCO 3 -MTBE, and SPME) based on gas chromatography-mass spectrometry (GC-MS) analysis. The specificity, linearity, recovery, precision, and sensitivity of different analytical approaches were systematically assessed using SCFA chemical standards and further validated with human fecal samples, ensuring cross-species applicability. Our results revealed that no single method performed optimally for all SCFAs, but rather, distinct methods exhibited compound-specific advantages. Moreover, this study provides a practical guideline for balancing recovery, reproducibility, and extraction efficiency for method selection based on research purposes. The H 3 PO 4 -Butanol method displayed superior recovery accuracy for valeric acid (100.16 ± 0.81% and 101.82 ± 4.83% recovery rate for low and median spiked concentrations, respectively). It also exhibited minimum intra-day repeatability (0.92% to 5.67% RSD values) and good linearity (R 2 =0.94-0.99) across chemical mixtures. However, it showed the best extracted efficiency for butyric acid and best sensitivity for isobutyruc acid in fecal samples. Moreover, the H 3 PO 4 -EA method showed the highest recovery accuracy for isobutyric acid (103.21 ± 11.07% to 104.79 ± 3.59% recovery rate for all three different spiked concentrations) and the smallest inter-day repeatability (3.37% to 7.25% RSD values). The SPME method exhibited superior recovery accuracy for acetic acid (81.16 ± 21.17% to 94.08 ± 10.92% recovery rate for all three different spiked concentrations) and extracted the highest levels of SCFAs for acetic acid, propionic acid, and isobutyric acid. Finally, the application of these methods in human clinical samples revealed significant alterations of SCFA levels in patients with missed abortion, supporting their potential for translational studies. Overall, our results indicated that H 3 PO 4 -Butanol and SPME are the recommended methods for studying SCFAs in fecal samples.
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PubMed
高影响因子
Food Chemistry-X
·
2023
·
IF 6.1
Huan Liu,Jingyu Li,Nazimah Hamid,Junke Li,Xuemei Sun,Fang Wang,Dengyong Liu,Qianli Ma,Shuyang Sun,Hansheng Gong
Smoked duck is a popular meat product in China. The aroma profile and key aroma compounds in smoked ducks were elucidated using solvent-assisted flavor evaporation-gas chromatography–olfactometry-mass spectrometry (SAFE-GC-O-MS), odor activity values (OAVs), aroma recombination and omission experiments, and sensory evaluation. The results indicated that the predominant aroma profiles of rice-, tea oil- and sugarcane-smoked ducks all contained strong smoky, roasty, fatty, meaty, and grassy aromas. A total of 31 aroma compounds were identified as important odorants by OAVs, including 8 aldehydes, 6 pyrazines, 5 phenols, and 2 sulfur compounds. The aroma recombination and omission experiments confirmed that 13 odorants were key aroma compounds in smoked ducks. Of these odorants, 2-methoxyphenol, 4-methylphenol, 5-ethyl-2,3-dimethylpyrazine, methional, 2-methyl-3-furanthiol, ( E, E )-2,4-decadienal, 1-octen-3-ol, and anethole significantly contributed to the aroma profile of smoked duck flavor ( p < 0.01).
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MOLECULES
·
2023
·Vol. 28
·期 5
·2205
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IF 4.6
Shengli Shi,Xinsha Zhang,Xianbin Liu,Zhen Chen,Hewen Tang,Dongbao Hu,Hongmei Li
The essential oil (EO) was extracted from aerial parts with insecticidal and fungicidal activity. Herein, the hydro-distilled essential oils ofSeseli maireiH. Wolff roots were determined by GC-MS. A total of 37 components were identified, (E)-beta-caryophyllene (10.49%),β-geranylgeranyl (6.64%), (E)-2-decenal (6.17%) and germacrene-D (4.28%). The essential oil ofSeseli maireiH. Wolff had nematicidal toxicity againstBursaphelenchus xylophiluswith a LC50value of 53.45 μg/mL. The subsequent bioassay-guided investigation led to the isolation of three active constituents: falcarinol, (E)-2-decenal, and octanoic acid. The falcarinol demonstrated the strongest toxicity againstB. Xylophilus(LC50= 8.52 μg/mL). The octanoic acid and (E)-2-decenal also exhibited moderate toxicity againstB. xylophilus(LC50= 65.56 and 176.34 μg/mL, respectively). The LC50of falcarinol for the toxicity ofB. xylophiluswas 7.7 and 21 times than that of octanoic acid and (E)-2-decenal, respectively. Our findings demonstrate that the essential oil fromSeseli maireiH. Wolff roots and their isolates may be developed as a promising natural nematicide.Keywords:Seseli maireiH. Wolff;Bursaphelenchus xylophilus;falcarinol
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Food Analytical Methods
·
2018
·Vol. 11
·期 9
·2628-2635
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IF 2.245
Qin Guofu,Zou Keting,Tian Li,Li Yongbo
An efficient and sensitive analytical method for the simultaneous determination of five plant growth regulators (PGRs) has been successfully developed, including 3-Indoleacetic acid (IAA), 2-Naphthylacetic acid (2-NAA), Beta-indolebutyric acid (IBA), 2-(2,4-dichlorophenoxy), acetic acid (2.4-D), and 4-Chlorophenoxyacetic acid (4-CPA) in bean sprouts. Using 10% boron trifluoride of methanol as the derived reagent and the reaction was derivatized at 70 °C for 30 min, the derivatives of five PGRs have been completely separated within 19 min. It has a linear relationship in the concentration range of 0.01–0.20 mg/kg and the correlation coefficients ( r 2 ) in excess of 0.997. The average recoveries were ranged from 72.7–98.6% at three spiking different concentration levels of 0.05, 0.10, and 0.15 mg/kg, respectively. The relative standard deviations (RSDs) were ranged from 1.2 to 9.0%. The limits of detection and the limits of quantification were ranged from 0.00024 to 0.00172 mg/kg and 0.0008–0.0052 mg/kg, respectively. On the basis of these, the measurement has been successfully applied to the analysis of the exogenous phytohormones in the bean sprouts. Except for 4-CPA and IAA, the rest of the analytes were undetected in samples. In sum, the current method can be used for accurate determination and confirmation of PGRs in many other crops, such as bean sprouts.
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MICROCHEMICAL JOURNAL
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2023
·
IF 4.8
Na Wang,An Gu,Guanghua Li,Yong Lei
Boiled tung oil is the commonly used drying oil in Chinese cultural relics, and light radiation, temperature are the important factors leading to its aging. In order to investigate the photo and thermal aging behavior of boiled tung oil and determine the characteristic parameters to evaluate its aging degree, micro-UV/Py-GC/MS system has been applied in the present work to monitor the volatile aging products released by boiled tung oil film, to obtain high aging degree boiled tung oil film in short time and to investigate its composition change in different aging degree. Research results showed that volatile products released by boiled tung oil film during UV irradiation and 60 ℃ were mainly series of aldehydes, ketones, carboxylic acids and hydrocarbons with small molecule. With increase of aging time, the type of volatile products remain unchanged, but their amount gradually decreases until cannot be detected. Pyrolytical products of unaged and aged boiled tung oil is the same, but with the increase of aging degree, relative content of glycerol, dicarboxylic acids and azelaic acid in boiled tung oil film gradually increased, while the relative content of oleic, linoleic and eleostearic acid, as well as the content ratio of mono-carboxylic acids to di-carboxylic acids gradually decreased. Changes of volatile and pyrolytical products during aging process were summarized to evaluate the aging degree of boiled tung oil used in cultural relics. Boiled tung oil used in two lacquerware samples collected from the same carved lacquer panel from Fuwang Ge in the Forbidden City, and two polychrome samples separately collected from the inner and outer eave of Yanxi Tang in the Forbidden City were investigated, the aging degree evaluation results of boiled tung oil in historical samples have further confirm the reliability of summarized parameters. Research results of the present work can provide scientific support for the conservation and restoration of related cultural relics, and also lay a foundation for the in-depth study of the photo and thermal aging mechanism of boiled tung oil.
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LWT-FOOD SCIENCE AND TECHNOLOGY
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2023
·
IF 6
Quanzeng Wei,Juntao Sun,Jiaqi Guo,Xiaofei Li,Xiaohua Zhang,Fugang Xiao
The adulteration of the honey industry is serious, especially the syrup adulteration method is difficult to detect. To develop the detection technology of chaste honey adulteration with high fructose corn syrup (HFCS), the condition of headspace solid-phase micro-extraction (HS-SPME) was optimized for extracting the volatile compounds of chaste honey. HS-SPME conditions were selected for optimization using Plackett Burman, steepest ascent and Box-Behnken. Volatile compounds from chaste honey adulterated with HFCS were analyzed by gas chromatography-mass spectrometry (GC-MS). M/Z RT pairs data from differences in chaste honey contents in HFCS-adulterated samples were analyzed by linear discriminant analysis (LDA), principal component analysis (PCA), and artificial neural network (ANN). The results indicated distinguished adulterated chaste honey at different proportions was not ideal using LDA and PCA. A back propagation (BP) artificial neural network （ANN）model was constructed based on m/z RT pair data. Correlation coefficients of training, verification, testing and comprehensive data of BP-ANN were 0.994, 0.945, 0.968 and 0.979, respectively, indicating good accuracy of the BP-ANN prediction model. The present study discusses a new strategy that determined the chaste honey contents in HFCS-adulterated samples as well as did not rely on the identification of volatile compounds.
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MACROMOLECULAR MATERIALS AND ENGINEERING
·
2022
·Vol. 307
·期 7
·2100948
·
IF 4.402
Jinbiao Min,Zhaoxi Zhou,Jia Zheng,Caibin Yan,Hongyuan Sha,Maochun Hong,Heqing Fu
In this paper, PVA/PAA-PAM-IS/GC composite hydrogels are prepared using polyvinyl alcohol (PVA), poly acrylic acid (PAA), poly acrylamide (PAM), and iron sulfate hydrate (IS) glycerol (GC). The crosslinking network is formed by the coordination of carboxyl groups with ions, which forms PVA with semi-interpenetrating network. The mechanical properties and self-healing properties of PVA/PAA-PAM-IS/GC composite hydrogels are excellent. The stress, strain and self-healing efficiency of PVA/PAA-PAM-IS/GC composite hydrogels can reach 840 kPa, 784%, and above 95%, respectively. The antifreeze and water retention properties of PVA/PAA-PAM-IS/GC composite hydrogels are improved by glycerol. PVA/PAA-PAM-IS/GC composite hydrogels remains flexible at low temperatures and moist for a long time at room temperature. The conductivity of the hydrogel increases with the increase of temperature because the interactions between glycerol, water molecules and ammonium ions are affected by the temperature, the multifunctional conductive hydrogel can be used in strain sensing and temperature sensing. In summary, PVA/PAA-PAM-IS/GC composite hydrogels can provide a guide in the field of electronic intelligence.
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LWT-FOOD SCIENCE AND TECHNOLOGY
·
2022
·
IF 6.056
Xia Yin,Jian'an Huang,Jing Huang,Wenliang Wu,Tong Tong,Shujuan Liu,Lingyun Zhou,Zhonghua Liu,Shuguang Zhang
Hunan black tea is well-known for its floral-honey aroma, but the volatile components responsible for the fragrance have not been elucidated yet. In this study, the volatile compounds in Hunan black tea were identified and quantified by the headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS). The results showed that 88 compounds were extracted and determined in Hunan black tea, including the dominant components Geraniol, phenethyl alcohol, phenylacetaldehyde, linalool, nonanal and other 5 aromatic compounds. Furthermore, the aroma-active compounds were identified by odor activity value (OAV). It was found that 24 aroma compounds, including geraniol with an OAV≥1 were regarded as the primary active aromatic compounds in Hunan black tea. Finally, partial least squares (PLS) regression analysis was employed and results revealed that Nonanal, trans -nerolidol, benzyl alcohol, and phenylethanol exhibit a positive correlation with the intensity of floral and sweet honey aromas. Overall, this study identified the volatile compounds responsible for the dominant floral-honey aroma in Hunan black tea.
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JOURNAL OF FOOD PROCESSING AND PRESERVATION
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2021
·Vol. 45
·期 3
·e15267
·
IF 2.19
Yuan-Hui Wang,Jing-Wen Zhao,Fei Xu,Qi-Dong Zhang,Zhi-Lu Ai,Bo-Yu Li
The volatile compounds of Jiaozi-steamed breads (JSBs) fermented by Jiaozi starters from eight regions in China were extracted using simultaneous distillation and extraction (SDE) and headspace solid-phase microextraction and determined using gas chromatography-mass spectrometry (GC-MS). 1-Hexanol, 3-methyl-1-butanol, phenylethyl alcohol, benzaldehyde, naphthalene, ethanol, acetic acid, and n -hexadecanoic acid were the main volatiles of JSBs. Principal component analysis exhibited that the volatiles of JSBs from Nanyang City, Xi'an City, and Zhumadian City was negatively correlated to that of other five JSB samples. Cluster analysis demonstrated that the volatile characteristics of JSBs from Heze City, Minqin County, Taian City, Weinan City, and Yuncheng City belonged to a category, and the JSBs of Nanyang City, Xi'an City, and Zhumadian City were different from other five JSBs. It demonstrated that the volatile components of steamed breads in North China and South China were different. Practical applications From this study, it can be seen that simultaneous distillation and extraction (SDE) can completely extract volatile compositions of steamed breads fermented by Chinese traditional starter “Jiaozi.” SDE/GC-MS was suitable for the analysis of JSBs volatile composition. The relative contents of 1-hexanol, 3-methyl-1-butanol, phenylethyl alcohol, benzaldehyde, naphthalene, ethanol, acetic acid, and n -hexadecanoic acid in JSBs were at high level, and their contents could be used as a marker to identify JSBs. The volatile compositions of JSBs made of Jiaozi starters from Heze City, Minqin County, Taian City, Weinan City, and Yuncheng City were similar. However, JSBs of Nanyang City, Xi'an City, and Zhumadian City were different from other five JSBs. The volatile components of steamed breads in North China and South China were different, which reflected the difference in dietary habit in the southern and northern areas of China.
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APPLIED SURFACE SCIENCE
·
2020
·
IF 6.182
Juan Xiong,Zhen Xiang,Baiwen Deng,Mengchen Wu,Lunzhou Yu,Zhicheng Liu,Erbiao Cui,Fei Pan,Rui Liu,Wei Lu
Designable microstructure was crucial for fabricating electromagnetic wave (EMW) absorbing materials. Herein, NiCo nanoparticles/graphitic carbon/nanoporous carbon (NiCo/GC/NPC) core–shell nanocomposites with novel hierarchical double yolk-shell structure were synthesized from metal-organic frameworks by a facile process. The yolk-shell nanoporous core–shell structure of the NiCo/GC/NPC nanocomposites was expertly tuned by regulating the composition of the Ni and Co elements, leading to the engineering relaxation polarization, conductive loss, magnetic resonance and multiple scatterings and reflections. The Ni 1 Co 2 /GC/NPC nanocomposite exhibited a minimum reflection loss ( RL min ) value of −52.2 dB and a broad effective absorbing bandwidth (EAB) of 7.2 GHz (from 10.8 to 18 GHz) for RL < −10 dB with a thin thickness of 2.1 mm. The outstanding absorbing performance was ascribed to the optimized nanostructure which integrated the yolk-shell configuration, nanoporous structure and core–shell architecture, which brought in higher tunable dielectric and magnetic loss with the good impedance matching. This work provides a facile paradigm for the design and fabrication of the yolk-shell nanoporous core–shell structure for light weight and high-efficiency EMW absorbers.
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危险品化学品经营许可证（带存储）