Analytical Methods
·
2014
·Vol. 7
·期 3
·1036-1045
·
IF 1.938
Xiaozhi Wang,Weijun Zhao,Lingfeng Li,Xiangyang Wang,Peng Li,Yu Wang,Jikui Luo
Sulfites (sulfur dioxide) and inorganic sulfites are types of food additives and preservatives, widely used in the production of food and herbal medicines (HMs). However, the overingestion of sulfites and its associates are harmful to human health and may cause medical complications. Various methods and instruments have been developed for measuring sulfites in foods and HMs, but they typically suffer from many issues, such as high detection limitation, inaccurate and non-reliable results, time and labor-intensive sample preparation, and high cost. Herein, we present a fast, sensitive, and quantitative method to determine sulfites in HMs using field asymmetric-wave ion mobility spectrometry (FAIMS) coupled with a headspace bubbling method. The headspace air bubbling method is effective and efficient at generating stable sulfur dioxide (SO2) in the gas phase for FAIMS analysis. It allows sulfites with a concentration down to 1 mg kg−1 to be easily detected by this new method in 20 min, much shorter than with current technologies. The limits of detection (LOD) and limits of quantification (LOQ) are 1 mg kg−1 and 3 mg kg−1 in HMs, respectively. The new method is of great significance to ensure medical safety and for HM production quality control.
研究领域:
分析化学
·
药学
·
食品安全
✓ 已验证
产品关联
DOI
高影响因子
Journal of Analytical Methods in Chemistry
·
2024
·
IF 2.3
Yajie Hao,Guang Yin,Xuemei Wang,Juan Fu,Qihui Cao,Qinyong Sun,Guimin Zhang,Zhong Feng
Rosuvastatin calcium is a widely used 3-hydroxy-3-methylglutaryl coenzyme A-reductase inhibitor developed for the treatment of dyslipidemia. To establish a control strategy for the elemental impurities, a new digestion method combined with an inductively coupled plasma-mass spectrometer (ICP-MS) was developed and validated by our team to determine elements Cd, Pb, As, Hg, Co, V, and Ni in rosuvastatin calcium tablets, which digest the sample perfectly even in the presence of a large number of excipients, especially titanium dioxide. The measurement mode was collision cell mode with kinetic energy discrimination (KED). 209Bi+, 115In+, and 89Y+ were chosen as internal standard elements. The recoveries of the limit of quantitation (LOQ) ranged from 90.5% to 106.4%, concentrations of the abovementioned elements in LOQ were 0.25 µg·L−1, 0.25 µg·L−1, 0.75 µg·L−1, 1.5 µg·L−1, 2.5 µg·L−1, 5 µg·L−1, and 8 µg·L−1 , respectively, linear correlation coefficients were above 0.9997, the recoveries in accuracy item ranged from 91.8% to 103.6%, and relative standard deviations (RSDs) of recovery in precision were not more than 1.8%, reflecting a reliable method of high sensitivity, strong anti-interference capacity, and good precision, and that it was suitable for the determination of elemental impurities in drugs.
研究领域:
药学
·
分析化学
✓ 已验证
DOI
PubMed
高影响因子
Journal of Cotton Research
·
2024
·Vol. 7
·期 1
·1-14
·
IF 3.1
Wang Wenhao,Song Xianpeng,Wang Dan,Ma Yajie,Shan Yongpan,Ren Xiangliang,Hu Hongyan,Wu Changcai,Yang Jun,Ma Yan
Background Plant hormones profoundly influence cotton growth, development, and responses to various stresses. Therefore, there is a pressing need for an efficient assay to quantify these hormones in cotton. In this groundbreaking study, we have established QuEChERS-HPLC‒MS/MS method, for the simultaneous detection of multiple plant hormones in cotton leaves, allowing the analysis and quantification of five key plant hormones. Results Sample extraction and purification employed 0.1% acetic acid in methanol and C18 for optimal recovery of plant hormones. The method applied to cotton demonstrated excellent linearity across a concentration range of 0.05–1 mg·L −1 , with linear regression coefficients exceeding 0.99. The limits of quantification (LOQs) were 20 μg·kg −1 for GA 3 and 5 μg·kg −1 for the other four plant hormones. Recovery rates for the five plant hormones matrix spiked at levels of 5, 10, 100, and 1000 μg·kg −1 were in the range of 79.07% to 98.97%, with intraday relative standard deviations (RSDs) ranging from 2.11% to 8.47%. The method was successfully employed to analyze and quantify the five analytes in cotton leaves treated with plant growth regulators. Conclusion The study demonstrates that the method is well-suited for the determination of five plant hormones in cotton. It exhibits excellent selectivity and sensitivity in detecting field samples, thus serving as a robust tool for in-depth research into cotton physiology.
研究领域:
农业化学
·
植物生理学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2021
·Vol. 60
·期 7
·705-711
·
IF 1.618
Huang Yang,Jiang Zhengjin
Saccharides are one of the most important biomoleculars in the world, which are responsible for various roles in living organisms. In this work, a combined use of mass spectrometry (MS) together with supercritical fluid chromatography (SFC) was applied for the separation of eight saccharides. A satisfactory separation was achieved within 15 min on a Unitary Diol column using 10 mM ammonium acetate in methanol as mobile phase additive at a temperature of 60°C. Compared to liquid chromatography–MS (LC–MS), the SFC–MS presented faster running time and better selectivity. The SFC–MS was validated and applied to the analysis of three saccharides (fructose, glucose and sucrose) present in different honey samples. The limits of detection (LODs) and limits of quantification (LOQs) of SFC–MS method for fructose, glucose and sucrose were 5.2, 4.5, 7.4 μg/mL and 17.2, 14.9, 24.1 μg/mL, respectively. The relative standard deviations for intrabatch and interbatch precision were <2.5% and the recoveries ranged from 97.6% to 103.1% for three concentration levels. The values of LODs and LOQs using SFC–MS method were lower (1.5–2.4-fold) than using LC–MS method. The results demonstrated the potential of SFC–MS for fast and sensitive determination of saccharides in honey.
研究领域:
分析化学
·
食品科学
✓ 已验证
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2018
·Vol. 81
·期 9
·1317-1323
·
IF 1.401
Zhang Chaozheng,Tang Ping,Xu Huijing,Weng Yanru,Tang Qiaoqiao,Zhao Hua
The level of short-chain fatty acids (SCFAs) is related to health benefits. In this study, a static headspace (HS) gas chromatography method was developed and validated for analyzing SCFAs in fecal samples. SCFAs were injected onto a column through an HS injector through an HS procedure and salting-out technology. The limits of detection and quantification (LOQ) of this method are 0.02–0.08 µg L − 1 (0.4–1.6 µg g − 1 sample) and 0.005–0.020 µg L − 1 (0.1–0.4 µg g − 1 sample), respectively. The calibration curves show good linearity over the range (LOQ–200 µg L − 1 or LOQ–4000 µg g − 1 sample) of these compounds, and the correlation coefficient is > 0.99. The recovery of the method is between 80 and 105%, and matrix effects were not observed. The proposed method was successfully applied to analyze SCFAs in fecal samples from rats. Graphical Abstract
研究领域:
分析化学
·
肠道微生物组学
·
营养学
✓ 已验证
DOI
高影响因子
ENVIRONMENTAL SCIENCE AND POLLUTION RESEARCH
·
2022
·Vol. 30
·期 10
·27357-27371
·
IF 5.19
Ma Qing-guang,Wan Yi-ping,Liu Ze-hua,Dang Zhi
Analytical method for three natural estrogens (NEs) and their sulfate and glucuronide conjugates in waste and river waters using solid-phase extraction (SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) has been available, but problems including poor recovery exist. In order to solve these, some optimizations have been performed in this work. For sample preparation, both rinse and elution solutions were optimized, in which 6 mL of MeOH/water (1:9, v/v), MeOH/Ace/water (10:2:88, v/v/v), and MeOH/NH 4 OH/water (10:2:88, v/v/v) were determined as the rinse solution, while 6 mL of 2.0% NH 4 OH/MeOH was determined as the elution solution for conjugated NEs (C-NEs). For mobile phase, addition of NH 4 F could obviously enhance the signal response of the nine target compounds, and the optimized addition concentration was 0.5 mmol/L. The developed efficient method was validated and showed excellent linearity for each target compound ( R 2 > 0.998), low limit of quantifications (LOQs, 0.07–1.29 ng/L) in four different water matrices, and excellent recovery efficiencies of 81.0–116.1% in influent, effluent, ultra-pure, and river water samples with low relative standard deviations (RSDs, 0.6–13.6%). The optimized method was successfully applied to influent, effluent, and Pearl River water, among which three NEs were all detected, while five C-NEs were found in the influent, three C-NEs were detected in the effluent, and two C-NEs were found in the Pearl River water, indicating the wide distribution of NEs and C-NEs in different water environments. This work provided a reliable and efficient analytical method for simultaneous trace determination of NEs and C-NEs, which had satisfactory absolute recoveries with low RSDs, low LOQs, and time-saving for both analysis and nitrogen drying.
研究领域:
环境科学
·
分析化学
·
水质
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
·
2023
·
IF 4.3
Ling Li,Ping Li,Shi Tang,Caiju Xiao,Yukun Huang,Lijun Wang,Xiao Yang,Xianggui Chen,Bing Shao
An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the simultaneous analysis of acrylamide (AA), 5-hydroxymethylfurfural (HMF), and heterocyclic aromatic amines (HAAs). A good separation of nine analytes was achieved within 15 min. Correlation coefficients (R 2 >0.9995) of the nine compounds were obtained within their respective linear ranges. The method also possessed low limits of detection (0.3 ng/mL for IQ, Norharman, 7,8-DiMeIQ, 10.00 ng/mL for MeIQ, 5-HMF, 0.05 ng/mL for PhIP, Phe-P-1, 0.10 ng/mL for Harman, 20.00 ng/mL for AA) and limits of quantification (15.00 mg/kg for IQ, Norharman, 7,8-DiMeIQ, 450.00 mg/kg for MeIQ, 3.00 mg/kg for PhIP, Phe-P-1, 300.00 mg/kg for 5-HMF and 750.00 mg/kg for AA). The method developed for the determination of samples commonly found among Sichuan cuisine, and fast food had good precision (RSD<9%) and recovery (83%-113%). This study provides a basis for the simultaneous rapid determination of nine chemical contaminants commonly found in thermally processed meat products and provides a technical reference for the simultaneous rapid determination of more chemical contaminants in thermally processed meat products.
研究领域:
分析化学
·
食品科学
·
毒理学
✓ 已验证
产品关联
DOI
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
JOURNAL OF MASS SPECTROMETRY
·
2022
·Vol. 57
·期 2
·e4809
·
IF 2.394
Gaosheng Zhao,Fengjian Chu,Jianguang Zhou
A direct analytical method based on dual ambient plasma ion source tandem mass spectrometry was used for the simultaneous determination of four sterols in the environment. This technology has very high sensitivity and the method detects the four sterols in methanol–water (1:3) solutions with limits of detection (LOD) and limits of quantification (LOQ) ranging from 1.2 ng/L to 6.9 ng/L and 7.6 ng/L to 10.0 ng/L, respectively. The method was also used to test water quality at three locations within the city and successfully detected all four sterols at very low concentrations. The dual plasma source tandem mass spectrometry technique is extremely simple, rapid, sensitive and highly efficient compared to other traditional methods, providing a useful screening tool for sterols in water.
研究领域:
环境科学
·
分析化学
·
水质监测
✓ 已验证
DOI
PubMed
高影响因子
SN Applied Sciences
·
2019
·Vol. 2
·期 1
·1-11
·
IF 0
Li Genrong,Yu Wenqin,Xiao Zhaojing,Long Mei,Tong Lanyan,Qiu Yue
A rapid, sensitive, and practical QuEChERS method coupled with gas chromatography–mass spectrometry was developed for the simultaneous determination of 16 chemical adjuvant residues in samples of fruits (apple, nectarine, grape) and vegetables (tomato, cucumber, spinach). All target compounds were separated in less than 16 min. Samples were extracted with acetonitrile, and the types of extraction salt and cleanup sorbent were optimized. The optimized method was validated by evaluating the linearity, accuracy, precision, and matrix effect. The recoveries of the 16 pesticides adjuvants ranged from 61.2 to 116.3% with relative standard deviations lower than 11.6%. Limits of detection ranged from 0.21 to 3.02 μg/kg, and limits of quantification ranged from 0.71 to 10.07 μg/kg. Finally, the developed method was successfully employed to identify and quantify pesticide adjuvant residues in the analysis of 30 real fruit and vegetable samples.
研究领域:
分析化学
·
食品科学
·
环境科学
✓ 已验证
产品关联
DOI
RSC Advances
·
2015
·Vol. 5
·期 102
·84164-84171
·
IF 3.84
Guifang Du,Xiaomei Yang,Mu Hu,Chengcheng Hao,Yanan Gu,Xiuyi Zhi,Wen G. Jiang,Junqi He,Shan Cheng
NHERF1 might play a significant role in biological processes including oncogenic transformation and metastasis. Owing to the lack of highly sensitive and quantitative methods of NHERF1 in human plasma, there have been few reports on the plasma levels of NHERF1 and its correlation with cancer. Here, a novel amplified luminescent proximity homogeneous immunoassay (AlphaLISA) has been developed and validated for the quantification of NHERF1 in human plasma. This assay was based on an AlphaScreen detection technique with two different anti-NHERF1 antibodies coupled to donor and acceptor beads, respectively. The developed AlphaLISA assay was further optimized and validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), precision, recovery, selectivity and interferences. The linear range of NHERF1 in human plasma was 5.00–100 ng mL−1, with an LOD of 2.00 ng mL−1. This AlphaLISA assay has been successfully applied to the quantification of NHERF1 in the plasma from 75 patients with non-small cell lung cancer (NSCLC). The levels of NHERF1 protein in plasma from patients with NSCLC were significantly higher than those in the healthy group (p = 0.0004). Based on the evaluation of the ROC curves, measuring the content of NHERF1 in human plasma could provide a potential diagnostic tool for NSCLC.
研究领域:
肿瘤学
·
分子生物学
·
临床化学
·
癌症生物标志物
✓ 已验证
产品关联
DOI
高影响因子
ANALYTICAL SCIENCES
·
2023
·
IF 1.6
Zhang Miaomiao,Wei Xuanwen,Bai Ligai,Liu Haiyan
In present work, a method for enrichment, purification, and content determination of oleanolic acid (OA) in medicinal plants was established based on on-line solid phase extraction (SPE). A metal organic frameworks–porous organic polymer monolith (MOF–POPM) was prepared with functionalized UiO-66-(OH) 2 as monomer and was used as SPE column for online enrichment and purification of OA. The ratio of adsorbent, enriching and eluting solvent, mobile phase pH, and flow rate had been systematically investigated. Under the optimum conditions, the linear range of OA was 0.59–2500 μg/mL with r = 0.9996. The limit of detection (LOD) was 0.18 μg/mL and the limit of quantification (LOQ) was 0.59 μg/mL. The intra-day relative standard deviations (RSDs) and inter-day RSDs of retention time and peak area were less than 0.3% and 1.3%, respectively. The average recoveries of OA in medicinal plants samples ranged from 87.7 to 104.6%. The results demonstrated that the online system was reliable and accurate for enrichment, purification, and content determination of OA in medicinal plants. Graphical abstract
研究领域:
分析化学
·
药学
·
材料科学
✓ 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）