Toxins
·
2024
·Vol. 17
·期 1
·11
·
IF 3.9
Hui-Qin Pan,Rui Feng,Yan-Nan Tan,Xiao-Ya Qin,Yi-Min Cao,Xiu-Hong Mao,Qing Hu,Heng Zhou
Puberulic acid (PA) is a mycotoxin produced by a species ofPenicillium. It has received widespread attention as a significant contributor to the reported fatalities associated with red yeast rice dietary supplements. However, the detection of PA, especially at low concentration levels, poses a considerable challenge, with no detection methods reported thus far. Here, we present a simple and sensitive derivatization-based LC-MS/MS method, requiring no purification processes, for determination of PA in the red yeast rice. The methylating derivatization with trimethylsilyldiazomethane (TMSCHN2) was performed to enhance its analytical performance. To achieve optimal detection sensitivity, the amount of solvent and TMSCHN2for the derivatization reaction, along with the reaction time, were individually optimized. Moreover, sample extraction solvent was carefully chosen to improve recoveries in real sample analyses. Comparatively, the proposed LC-MS/MS method achieved a superior detection sensitivity, over 100-fold higher than that of the liquid chromatography method. A good linear relationship within the concentration range of 5 ng/mL to 200 ng/mL (with a linear correlation coefficient of 0.99952) was demonstrated by the method validation. The average recovery rate was between 82.2% and 84.2%, and the repeatability (RSD of 2.1% to 10.4%, n = 6) was satisfactory. The derivatized PA remained stable within 48 h. The limit of detection and the limit of quantification could reach 2 μg/kg and 50 μg/kg, respectively. As a result, the method was successfully applied to detect PA in over 42 batches of the red yeast rice samples. It indicated a low risk of PA contaminations in the red yeast rice products made in China. Furthermore, its application to the other health food products containing red yeast rice demonstrated the applicability of the established method.
研究领域:
食品科学
·
分析化学
·
毒理学
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产品关联
DOI
PubMed
高影响因子
ADSORPTION SCIENCE & TECHNOLOGY
·
2020
·
IF 2.425
Qiaoling Xie,Gaojie Liang,Tao Lin,Fuming Chen,Dandan Wang,Bo Yang
A study on selective chelating precipitation of palladium metal from real electroplating wastewater using chitosan and its water-soluble derivative was conducted. The pH parameter, the concentrations of chitosan and its water-soluble derivative and the chelating precipitation time were experimentally investigated, and the optimum conditions were determined. The results revealed that both chitosan and its water-soluble derivative acted as chelating precipitation agents. Rapid chelating precipitation occurred when chitosan was added to real electroplating wastewater containing the chitosan derivative, thereby improving removal efficiency of palladium in different forms up to 95% under the optimum condition of 0.2 g/L chitosan and 0.16 mg/L derivative at pH 2.5. Then, dissolution experiments showed that chelating precipitation products could be dissolved in aqua regia. Additionally, selective chelating precipitation of palladium by chitosan and its derivative was characterized using X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy. Thus, it can be concluded that the combined utilization of chitosan and its water-soluble derivative is a promising approach method for the removal of different forms of palladium from real electroplating wastewater.
研究领域:
环境科学
·
材料科学
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES
·
2016
·
IF 2.687
Zhongyi Zhang,Jing Tian,Hongwei Xiao,Nengjian Zheng,Xiaofei Gao,Renguo Zhu,Huayun Xiao
The signatures of natural stable nitrogen isotopic composition (δ 15 N) of individual amino acid (AA) have been confirmed to be a potentially effective tool for elucidating nitrogen cycling and trophic position of various organisms in food webs. In the present study, a two-stage derivatisation approach of esterification followed by acylation was evaluated. The biological samples underwent acid hydrolysis and the released individual AA was derivatived into corresponding N -pivaloyl-isopropyl (NPIP) esters for nitrogen isotopic analysis in gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). Usually, 13 individual AA derivatives were separated with fine baseline resolution based on a nonpolar gas chromatography column (DB-5 ms). The minimum sample amount required under the presented conditions is larger than 20 ngN on column in order to accurately determine the δ 15 N values. The δ 15 N values determined by GC-C-IRMS with a precision of better than 1‰, were within 1‰ after empirical correction compared to the corresponding measured by element analysis (EA)-IRMS. Bland-Altman plot showed highly consistency of the δ 15 N values determined by the two measurement techniques. Cation-exchange chromatography was applied to remove interfering fraction from the extracts of plant and animal samples and without nitrogen isotope fractionation during the treatment procedure. Moreover, this approach was carried out to estimate the trophic level of various natural organisms in a natural lake environment. Results highly proved that the trophic level estimated via the presented AA method well reflected the actual food web structure in natural environments.
研究领域:
生态学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
FOOD RESEARCH INTERNATIONAL
·
2024
·
IF 7
Yun-Jiao Ma,Ping Li,Bei-Wei Zhu,Ming Du,Xian-Bing Xu
The comprehensive determination of fatty acids without derivatization, including short-chain fatty acids (SCFAs), medium-chain fatty acids (MCFAs) and long-chain fatty acids (LCFAs), is a big challenge but powerful for lipidomics in biology, food, and environment. Herein, the dual mode unity solid-phase microextraction (DMU-SPME) combined with gas chromatography-flame ionization detector (GC-FID) or mass spectrometry (MS) was proposed as a powerful method for the determination of comprehensive free fatty acids in real samples. Under the optimized DMU-SPME conditions, the proposed method has good linearity (R 2 ≥ 0.994) and low limits of determination (0.01–0.14 mg/L). In the stability analysis, the intra-day relative standard deviation was 1.39–12.43 %, and the inter-day relative standard deviation was 2.84–10.79 %. The recoveries of selected 10 fatty acids in real samples ranged from 90.18 % to 110.75 %, indicating that the method has good accuracy. Fatty acids ranging from C2 to C22 were detected in real samples by the untargeted determination method of DMU-SPME combined with gas chromatography-mass spectrometry (GC–MS). The DMU-SPME method proposed in this study can be used for lipid metabolism analysis and free fatty acid determination in the fields of biology, food, and environment.
研究领域:
生物化学
·
食品科学
·
环境科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
LWT-FOOD SCIENCE AND TECHNOLOGY
·
2016
·
IF 2.711
Xiaoqun Wei,Linzhou Zhuang,Chaomin Wu,Wenrui Chen,Zhiyong Li,Baojun Xu
A novel method for quantitative analysis of ethylenediaminotetracetic acid (EDTA) in wines and beers by liquid chromatography coupled to tandem mass spectrometry has been developed. Positive-ion mode was applied as the scan mode, amine species were firstly used as the derivatization reagents of EDTA, and phenylboronic acid was used to react with maltose to eliminate its matrix interference. Primary amines could efficiently eliminate the interference from metal ions (Fe(III) and Cu(II)). The responsive intensity of EDTA with amine derivatization could be improved over 300 times than that without adding amine species. The recovery rate was significantly increased to 104.1% after adding phenylboronic acid at 20.0 mg/L as compared to the control spike-and-recovery experiment results (1.3–1.7%) of beer samples without adding phenylboronic acid. The validated method showed excellent detection sensitivity (0.001 mg/L for LOD (limit of detection) and 0.004 mg/L for LOQ (limit of quantification)) with satisfactory recovery rates (76.0%–97.2%), and good precision (1.40–5.40% RSD values). The optimized method has been satisfactorily applied to the analysis of actual wine and beer samples. It can be proposed as a powerful analytical method of EDTA in wines and beers, and can even be adapted to detect other chelates and polydentate compounds.
研究领域:
分析化学
·
食品科学
✓ 已验证
DOI
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2022
·
IF 4.52
Qiuyu Lin,Jiannan Sun,Yuanchao Wang,Meiying Ye,Heyong Cheng
Due to endogenous existence and hazardous properties, the quantification of fatty and aromatic aldehydes in food matrices is indispensable to food safety. Current analytical methodologies for aldehydes in food suffer from several drawbacks (typically complicated pretreatment, long analysis time and low analytical throughput, low sensitivity, etc.). In this work, a highly sensitive, high-throughput and sample pretreatment-free method for aldehyde analysis was developed to address the above problems, where in situ extraction and derivatization of aldehydes with hydrazines to hydrazones were integrated into reactive paper spray ionization mass spectrometry (reactive PSI-MS) considering weakly ionizable properties of aldehydes. Four aldehydes, formaldehyde, acetaldehyde, propionaldehyde and benzaldehyde were reacted with dansyl hydrazine in 1.5 % v/v HAc acidified methanol on the qualitative fast-speed filter paper for 5 min, and then a voltage (+4 kV) was applied to initiate paper spray for mass spectrometry detection with internal calibration by dansyl amide. Once the completion of MS analysis , the glass plate was moved to introduce the second triangular tip towards the MS inlet (5 mm apart) for next trial, achieving high-throughput reactive PSI-MS analysis (60 h −1 ). The four aldehydes showed good linearity in the concentration range from 2 to 150 μM with low detection limits of 0.03–0.15 μM. The method was applied to direct quantification of four aldehydes in 15 kinds of foods such as vegetables, fruits and meat products. The proposed method has the advantages of simple operation, high efficiency and high sensitivity, making it attractive to routine analysis of aldehydes in food, environmental and biological samples.
研究领域:
分析化学
·
食品安全
·
质谱分析
✓ 已验证
DOI
高影响因子
Food Analytical Methods
·
2021
·Vol. 14
·期 6
·1099-1109
·
IF 3.366
Jin Yueying,Xu Chun-Yan,Wang Jing,Man Xiaoxi,Shi Qing,Nie Fenghuan,Nan Jun,Min Jun Zhe
A new simple and sensitive method for the simultaneous detection of free DL-amino acids (DL-AA) in natto was established by UPLC-fluorescence (FL) using the newly developed fluorescence derivatization reagent DBD-trans-2-methyl-L-proline (DBD-M-Pro) by precolumn derivatization. DBD-M-Pro reacts with DL-amino acids at 60 °C for 60 min. Using BEH C18 (2.1 mm × 100 mm, 1.7 μm) column gradient analysis for 20 min, the resolution of diastereomers after the derivatization of four DL-amino acids was 1.65–3.50. The detection limit for amino acids was 0.25–2.5 pmol. The average recovery (%) of DL-amino acids was 86.65–118.70%. The method was applied to the detection of chiral amino acids in natto beans and mucus, and four chiral amino acids, DL-Gln, DL-Asp, DL-Glu, and DL-Ala, were simultaneously detected. At the same time, the DL-amino acid content and D/L ratio of three different manufacturers of natto were compared quantitatively.
研究领域:
生物化学
·
食品科学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2018
·
IF 4.946
Si-Jin Liu,Juan-Juan Xu,Chang-Lu Ma,Chun-Feng Guo
The six biogenic amines in sausage and cheese were analyzed by HPLC with UV detection after off-line derivatization with dansyl chloride, 9-fluorenylmethoxycarbonyl chloride, benzoyl chloride and dabsyl chloride, respectively. The results showed that both the off-line 9-fluorenylmethoxycarbonyl and dabsyl derivatization were not suitable for HPLC analysis of biogenic amines when batch injection was used because the derivatives were instable, whereas both the off-line dansyl and benzoyl derivatization were suitable for HPLC analysis of biogenic amines when batch injection was used, but the latter needed to maintain the derivatives at 4 °C to ensure that benzoylated tyramine was not degraded when waiting for the analysis. The off-line dansyl derivatization had an obvious advantage in the analysis of biogenic amines in sausage and cheese samples by HPLC combined with batch injection because the method has a wider linear range and higher sensitivity, accuracy, precision and stability of the derivatives.
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
INTERNATIONAL JOURNAL OF BIOLOGICAL MACROMOLECULES
·
2018
·
IF 3.909
Baolei Fan,Tingting Li,Xiaofang Song,Chao Wu,Chunqi Qian
A specific HPLC-MS/MS (High-Performance Liquid Chromatography with tandem Mass Spectrometry) method was developed and validated for simultaneous determination of several monosaccharides in three kinds Osmanthus fragrans Lour . After extraction, separation, protein removal, pigment removal and hydrolysis , monosaccharides was finally obtained from Osmanthus fragrans Lour . Positive ion mode detection and Multiple Reaction Monitoring (MRM) mode were used for quantitative analysis by PMP pre-column derivatization and Electrospray Ionization (ESI). Analysis and content determination of 6 monosaccharide components in 3 kinds of Osmanthus fragrans Lour . The HPLC separation was achieved on a Shim-pack VP-ODS6022748 (150 L × 2.0) with gradient elution at a flow rate of 0.2 ml/min in a run time of 40 min, and the mobile phase was acetonitrile-5 mmol/L ammonium acetate. PMP derivatization in HPLC-MS/MS can accurately measure Osmanthus fragrans Lour . mannose (Man), ribose (Rib), rhamnose (Rha), galacturonic acid (Gal UA), glucose (Glu), galactose (Gal), xylose (Xyl), fucose (Fuc). The results showed that HPLC-MS/MS pre-column derivatization method was simple and rapid, with small measurement error, but high sensitivity and good repeatability. The analysis of monosaccharide components in polysaccharide components has important practical significance.
研究领域:
植物化学
·
分析化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
·
2024
·
IF 4.9
Wenqing Zhang,Hao Zhu,Wenjie Xie,Chuanyuan Du,Xiuqiang Fang,Ruiming Zhang,Xiaosong Hu,Yawei Lin
A novel fluorescent probe , 3-(4-((hydroxylamino)methyl)-1H-pyrazol-1-yl)-7-methoxyl coumarin (HAPMC), has been designed and synthesized. The compound exhibits exceptional fluorescence properties due to a coumarin-pyrazolyl fluorophore. Moreover, it incorporates an N -hydroxylamine functional group capable of reacting with aldehydes to yield nitrone derivatives under mild conditions. This unique combination renders it an ideal derivatization reagent for aldehyde analysis. A standard method was established for the quantitative analysis of eight fatty aldehydes by utilizing high-performance liquid chromatography with fluorescence detection (HPLC-FLD) and a pre-column derivatization process, which has low detection limits (0.3–1.2 nM), satisfactory reproducibility (intraday and interday relative standard deviations in the range of 1.29 %-2.92 % and 1.73 %-3.45 %), and an extensive linear range (25–5000 nM) with excellent linearity (R 2 ≥ 0.9989). The spiked recoveries of the fatty aldehydes range from 89.6 % to 106.0 %. The greenness and sustainability of our approach are reinforced by evaluations conducted with the AGREE and RGB 12 algorithms. The established method was successfully applied to the qualitative and quantitative detection of fatty aldehydes in nine real vegetable oil samples, including peanut, canola, rice, soybean, olive, rapeseed, corn, sunflower, and blended oils. The fatty aldehydes are known to have adverse effects on human health due to their carcinogenic and mutagenic properties. The findings revealed that hexanal and nonanal were the most prevalent saturated fatty aldehydes, with a notable increase in the total aldehyde concentration observed as the temperature and duration of heating increased. Compared to alternative analytical techniques, this pre-column derivatization method utilizing HAPMC displayed simplicity, reliability, and sensitivity. The results demonstrate the potential for broad application of this approach in various important research domains, including food quality control, environmental monitoring, and medical research.
研究领域:
食品科学
·
分析化学
·
医学研究
✓ 已验证
产品关联
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2012
·
IF 4.531
Kaoqi Lian,Pingping Zhang,Lingmei Niu,Siyuan Bi,Shipeng Liu,Lingling Jiang,Weijun Kang
A new method was developed for determination of ketamine (KT) in urine and plasma samples by derivatization and gas chromatography–mass spectrometry. In this article, KT was first derivatized with sodium nitrite to volatile N-nitrosamines under acidic condition. Then the derivative had been identified by the mass spectra. The derivatization conditions including the amount of hydrochloric acid, the amount of sodium nitrite, reaction temperature, reaction time and the extraction reagents were optimized. Calibration curves were linear in the range of 0.04–20 μg mL −1 for KT, and the limit of detection (LOD) and limit of quantitation (LOQ) were 0.01 μg mL −1 and 0.04 μg mL −1 , respectively. The results of recovery indicated that the method had good precision and reproducibility. Compared with existing derivatization methods, this method provided a rapid, convenient, effective and low-cost way for gas chromatography method of KT quantification.
研究领域:
分析化学
·
医学检验
✓ 已验证
DOI
PubMed
高影响因子
TALANTA
·
2015
·
IF 3.545
Jiu-Feng Liu,Bi-Feng Yuan,Yu-Qi Feng
In this study, magnetic solid phase extraction coupled with in - situ derivatization (MSPE-ISD) was established for the determination of hexanal and heptanal in human urine. 2,4-Dinitrophenylhydrazine (DNPH) was used as the derivatization reagent that was adsorbed onto the surface of magnetite/silica/poly(methacrylic acid-co-ethylene glycol dimethacrylate) (Fe 3 O 4 /SiO 2 /P(MAA-co-EGDMA)). And then simultaneous extraction and derivatization of the aldehydes were performed on the DNPH-adsorbed Fe 3 O 4 /SiO 2 /P(MAA-co-EGDMA). The simple, rapid and sensitive determination of hexanal and heptanal can be accomplished within 9 min. Under optimized conditions, the limits of detection (LODs) were 1.7 and 2.5 nmol/L for hexanal and heptanal, respectively. The relative recoveries ranged from 72.8% to 91.4% with the intra- and inter-day relative standard deviations (RSDs) being less than 9.6%. Furthermore, the proposed method was successfully applied to determine endogenous hexanal and heptanal in human urine from healthy persons and lung cancer patients. The results showed the higher concentrations of hexanal and heptanal were observed in lung cancer patients compared to healthy controls. Thus, the developed MSPE-ISD method is suitable for the determination of aldehydes in urines.
研究领域:
分析化学
·
医学诊断
·
生物标志物研究
✓ 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）