Toxicologie Analytique et Clinique
·
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
·
毒理学
·
临床医学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
·
2013
·
IF 2.947
Chen Li,Feng Xu,Chen Cao,Ming-Ying Shang,Cui-Ying Zhang,Jie Yu,Guang-Xue Liu,Xuan Wang,Shao-Qing Cai
Traditional Chinese medicines (TCM) can be identified by experts according to their odors. However, the identification of these medicines is subjective and requires long-term experience. In this paper, electronic nose, headspace gas chromatography–mass spectrometry (GC–MS) and chemometrics methods were applied to differentiate two species of Asari Radix et Rhizoma by their odors. The samples used were the dried roots and rhizomes of Asarum heterotropoides var. mandshuricum (AH) and Asarum sieboldii (AS). The electronic nose was used to determine the odors of the samples and enabled rapid differentiation of AH and AS when coupled with principal component analysis. Headspace GC–MS was utilized to reveal the differences between the volatile constituents of AH and AS. In all, 54 volatile constituents were identified, and 9 major constituents (eucalyptol, eucarvone, 3,5-dimethoxytoluene, 3,4,5-trimethoxytoluene, methyleugenol, 2,3,5-trimethoxytoluene, croweacin, pentadecane and asaricin) could be used as chemical markers to distinguish these two species. AH contained higher relative contents of eucarvone (1.79–16.76%), 3,5-dimethoxytoluene (6.64–26.52%), 3,4,5-trimethoxytoluene/methyleugenol (6.43–31.67%) and 2,3,5-trimethoxytoluene (1.64–6.66%), whereas AS had higher relative contents of eucalyptol (14.06–24.95%), croweacin (5.64–13.55%), pentadecane (8.44–20.82%) and asaricin (7.03–13.45%). Moreover, AH and AS could be distinguished according to the contents of either all 54 identified volatile constituents or only the 9 major constituents by employing cluster analysis. The proposed method is rapid, simple, eco-friendly and can successfully differentiate these two species of Asari Radix et Rhizoma by their odors.
研究领域:
中药鉴定
·
分析化学
·
天然药物化学
·
代谢组学
·
药用植物学
✓ 已验证
DOI
高影响因子
JOURNAL OF FOOD PROCESSING AND PRESERVATION
·
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.
研究领域:
食品科学
·
分析化学
·
微生物学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF FOOD BIOCHEMISTRY
·
2019
·Vol. 44
·期 1
·e13088
·
IF 1.358
Xiao Tian,Sen Guo,Shanshan Zhang,Peisheng Li,Tianyi Wang,Chi-Tang Ho,Min-Hsiung Pan,Naisheng Bai
The seeds of tree peony ( Paeonia ostii ) are promulgated as emerging edible oil crops. However, biological properties of principal constituents of peony seeds were not well studied. Fifteen main constituents including suffruticosols A and B, trans -ε-viniferin, ampelopsin E, resveratrol, trans -resveratrol-4′- O -β- d -glucopyranoside, paeoniflorin, luteolin, luteolin-4′- O -β- d -glucopyranoside, apigenin, kaempferol, oleanic acid, betulinic acid, hederagenin, and caffeic acid were isolated and identified. Their cytotoxicity against human tumor cell lines (COLO205, HT-29, HepG2, AGS, and HL-60) were evaluated. Among them, trans -ε-viniferin showed the most potent cytotoxicity against HL-60 cells (IC 50 5.6 μM); ampelopsin E exhibited the most obvious antiproliferative properties on COLO205 (IC 50 78.1 μM) and HT-29 (IC 50 4.2 μM) cells, and betulinic acid showed the strongest growth inhibitory effects on HepG2 (IC 50 6.6 μM) and AGS (IC 50 5.4 μM) cells. Three enzymes (tyronsinase, α-glucosidase, and acetylcholinesterase) inhibitory activities of 12 compounds were also screened. Stilbene compounds, especially suffruticosols A and B, showed a significant inhibitory activity on all three enzymes. Practical applications The cytotoxicity of 15 main constituents from peony seeds against COLO205, HT-29, HepG2, AGS, and HL-60 cells were evaluated. Among them, trans -ε-viniferin showed the most potent cytotoxicity against HL-60 cells (IC50 5.6 μM); ampelopsin E exhibited the most obvious antiproliferative properties on COLO205 (IC50 78.1 μM) and HT-29 (IC50 4.2 μM) cells, and betulinic acid showed the strongest growth inhibitory effects on HepG2 (IC50 6.6 μM) and AGS (IC50 5.4 μM) cells. Collectively, these results suggested that Paeonia ostii seed (POS) extracts are potential candidates for anticancer agents.
研究领域:
药理学
·
生物化学
·
癌症研究
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植物科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Food Analytical Methods
·
2018
·Vol. 11
·期 9
·2628-2635
·
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.
研究领域:
植物学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
CHROMATOGRAPHIA
·
2016
·Vol. 80
·期 1
·165-170
·
IF 1.332
Yu Tianxiao,Wang Teng,Huang Zhenglan,Huang Ningshu,Zhang Hui,Luo Zhenhong,Li Hui,Ding Shijia,Feng Wenli
Abstract Pesticides are often involved in numerous acute and fatal poisonings. Patients’ blood samples may be sent to a toxicological laboratory for a poisoning diagnosis. This study proposes a gas chromatography-mass spectrometry (GC–MS) method for the determination of seven pesticides (malathion, methyl isofenphos, dichlorvos, chlorpyrifos, phenthoste, p , p ′-DDD, p , p ′-DDE) in human blood based on a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation method with Fe 3 O 4 magnetic nanoparticles (MNPs) as the new adsorbing material. It proved that Fe 3 O 4 MNPs have excellent adsorbent function while purifying the complex blood sample and it is simple to be separated from the extract. Under the optimum conditions, the detection limits of the proposed method for seven pesticides ranged from 0.011 to 0.163 µg mL −1 . Good linearity ( R value ≥0.9949) was achieved at concentration levels of 0.3–4.0 µg mL −1 , and acceptable method recoveries were found in the range of 70.0–111.8% at different concentrations, with the relative standard deviations (RSD) less than 10.5%. In short, the QuEChERS method with Fe 3 O 4 MNPs used for removing impurities improved the speed of sample pre-treatment and exhibited an enhanced performance in purifying. It can be applied for both forensic and clinical cases of accidental or suicidal poisoning with these pesticides. Graphical abstract
研究领域:
分析化学
·
毒理学
✓ 已验证
产品关联
DOI
高影响因子
MICROCHEMICAL JOURNAL
·
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.
研究领域:
文物保护
·
分析化学
·
材料科学
✓ 已验证
产品关联
DOI
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
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.
研究领域:
食品科学
·
分析化学
✓ 已验证
产品关联
DOI
高影响因子
MOLECULES
·
2023
·Vol. 28
·期 5
·2205
·
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
研究领域:
植物化学
·
植物保护
·
药理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
ANALYTICA CHIMICA ACTA
·
2014
·
IF 4.517
Juan Zheng,Siyan Li,Ying Wang,Lei Li,Chengyong Su,Hong Liu,Fang Zhu,Ruifen Jiang,Gangfeng Ouyang
A superior solid-phase microextraction (SPME) fiber-coating material, IRMOF-3@ILs/PDMS, was prepared by the in situ growth of IRMOF-3 onto stainless-steel wires and protection with ionic liquids (ILs) and polydimethylsiloxane (PDMS). The ILs can efficiently prevent the substantial cracking of IRMOF-3 caused by moisture, and a thin PDMS film can protect the IRMOF-3@ILs material to achieve a much better extraction efficiency as well as excellent resistance to high temperature and high humidity. This IRMOF-3@ILs/PDMS coating possessed a porous structure, a rough surface and an increased lifespan (by at least 100 times) compared with that of IRMOF-3. The coating was evaluated by analyzing four polycyclic aromatic hydrocarbons (PAHs) in water, and good precision (<7.7%), low detection limits (12.0–15.4 ng L −1 ), and wide linearity (50–20,000 ng L −1 ) were achieved under the optimized conditions. The fiber was successfully applied to the sensitive analysis of PAHs in rainwater by coupling it with gas chromatography–mass spectrometry (GC–MS).
研究领域:
分析化学
·
环境科学
·
材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2024
·
IF 5.6
Kaili Yang,Li Xiao,Shishu Yang,Caixia Ji,Suling Feng,Shengrui Xu
A straightforward approach to fabricating robust and versatile solid-phase microextraction (SPME) fibers is crucial for the extensive research and application of this notable sample preparation technique. Herein, we proposed a strategy for preparation of oxidative polyacrylonitrile (O-PAN) and O-PAN/ZIF-67 nanofiber-based SPME coatings by wrapping an electrospinning membrane on the stainless-steel wire, following with thermal oxidation at 300 °C. The shrinkage of membrane during thermal treatment resulted in the nanofibers being securely affixed to the stainless-steel wire, thereby creating a robust nanofiber-based SPME fiber. Furthermore, the characterizations results indicated that the thermal oxidation significantly enhanced the generation of oxygen-/nitrogen-containing groups within the nanofibers, which were conducive to the adsorption for the analytes. Given the exceptional properties, the proposed O-PAN/ZIF-67 coating was applied to extract and analyze polychlorinated biphenyls (PCBs) pollutants coupled with GC-MS, and exhibited superior extraction performances. The proposed analytical method presented a wide linear range spanning concentrations from 0.5 to 2500 ng L −1 , with a low detection limit ranging between 0.029 and 0.093 ng L −1 . Additionally, it demonstrated good precision, as evidenced by a relative standard deviation of 4.5 %–8.1 %, and was effectively utilized for the analysis of real water samples. This study introduced a novel, simple, and versatile methodology for the fabrication of nanofiber-based SPME coatings, offering a significant advancement in the field.
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
PHARMACEUTICAL CHEMISTRY JOURNAL
·
2020
·Vol. 54
·期 2
·154-161
·
IF 0.538
Ying-Jiao Liu,Li-Juan Xie,Lan Xiao,Li-Min Gong,Ta-Si Liu,Nai-Hong Chen
Cinnamomum camphora Chvar. Borneol (CCCB) and Cinnamomum camphora Chvar. Cineol (CCCC) are two different chemical types of C. camphora . The clinical application of these chemical types of CC shows big differences, but sometimes they are confused because of the similarity of morphological features. To identify the two types of CC and to analyze the differences of compositions, their morphological characteristics were investigated by microscopic techniques and the chemical components were determined by GC-MS analysis and GC internal standard method. Distinguishing features of morphological characteristics were the shape, petiol, gland, and smell. Microscopic study of the transverse sections of leaves showed 13 – 15 columns xylem vessel in the leaves of CCCB, 11 – 13 columns xylem vessel, and more obvious and thicker cell walls of fiber cells in the leaves of CCCC. From this research, GC-MS analysis of essential oil of the leaves could provide mainly differential characteristics to distinguish between CCCB and CCCC. The total of 33 compounds were identified in the essential oil of CCCB leaves and the main component was d -borneol (55.11%), while d -borneol in CCCC leaves was not the main component and the amount of d -borneol might be related to the microstructure of gland. L(-)-camphor and d-borneol were quantitatively analyzed by GC with FID detector, using methyl salicylate as the internal standard. Each gram of the total essential oil contains 0.68 g of d -borneol in CCCB, and each gram of the total essential oil contains 0.150 and 0.015 g of L(-)-camphor in CCCB and CCCC, respectively, from Hunan province. Other habitats showed the same trend. This research was aimed to establish a method based on the microscopic, GC-MS, and GC techniques to identify and quantify CCCB and CCCC compositions, for providing scientific data to ensure with accuracy the origin of CCCB and CCCC plant material.
研究领域:
植物学
·
药物分析
·
中药学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）