Journal of Analysis and Testing
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2024
·Vol. 8
·期 1
·1-8
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IF 5.5
Tu Mengling,Zhang Wei,Zhu Yunxiao,Ma Wen,Li Xiao,Zhou Shukun,Li Hongmei,Li Xianjiang
Thiacloprid is the first-generation neonicotinoid insecticide, which is widely used in modern agriculture. Reference materials are essential for sound measurement and traceability of results in chemical analysis. Pure thiacloprid was comprehensively assessed by two orthonormal methods: mass balance (MB) and quantitative nuclear magnetic resonance spectroscopy (qNMR). From MB, its mass fraction value was 998.4 mg/g with the subtraction of structurally related impurities (99.87%), inorganic impurities (0.006 mg/g), water (0.33 mg/g), and volatile organic solvent (0 mg/g). To guarantee sufficient separation of structurally related purity, peak purity of thiacloprid was evaluated by five points of UV spectra. From the qNMR of hydrogen, its mass fraction value was 995.7 mg/g which was traced to the internal standard (methyl sulfone). Finally, the certified value was assigned to 997 mg/g, together with an expanded uncertainty of 3 mg/g ( k = 2). This high-purity thiacloprid can be applied to routine monitoring in agriculture and the food fields.
研究领域:
分析化学
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农业科学
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食品科学
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产品关联
DOI
高影响因子
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
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2018
·
IF 2.831
Teng-Fei Yuan,Juan Le,Yan Cui,Rui Peng,Shao-Ting Wang,Yan Li
Background Comprehensive serum sex hormone profiling is essential for monitoring the occurrence and development of many related diseases. However, the current methods for multi-class sex hormone detection were always lack of Standard Reference Material (SRM) certification and suffered from large sample consumption. For improvement, we developed a new liquid chromatography-tandem mass spectrometry (LC–MS/MS) method focused on SRM certification and minimization of serum consumption for simultaneous quantification of seven mainstream serum sex hormones including estrogens (estrone E1, estradiol E2 and estriol E3), androgens (testosterone T, androstenedione AD, dehydroepiandrosterone DHEA) and progestogens (progesterone P). Methods To achieve one-batch analysis, a straightforward strategy was designed and carefully optimized. Schematically, serum was firstly spiked with isotope-labeled internal standards. Then, liquid-liquid extraction was performed with methyl tert-butyl ether. After drying under nitrogen, dansyl chloride was introduced for derivatization. Finally, the mixture was submitted to LC–MS/MS for quantification. Results The limit of quantification was 0.005 ng/mL for E1, E2 and E3, 0.01 ng/mL for T, P and AD, 0.25 ng/mL for DHEA. Inter- and intra-assay CVs were less than 11.8%. The selectivity was proved satisfactory by interference spiking tests. With systematical SRM validation, the mean bias of −5.4 to 4.7% was observed, which indicated excellent method reliability. We found significant positive bias in chemiluminescence immunoassay (CLIA) detection comparing with current method, which promoted us to reconsider our previous results on sex hormone regulation in male patients with coronary atherosclerotic disease. After redetecting the related samples, modified and improved conclusions were proposed. Conclusions A LC–MS/MS method for multi-class serum sex hormone profiling was developed with SRM certification and minimized serum consumption. Taking advantages of such reliable method, the previous CLIA-based research findings on sex hormone regulation in male patients with coronary atherosclerosis were modified and improved after redetecting the same sample-pool.
研究领域:
医学检验
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内分泌学
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临床化学
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DOI
PubMed
高影响因子
ANALYST
·
2022
·Vol. 147
·期 24
·5633-5642
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IF 5.227
Haijiao Dong,Guancheng Wang,Kaizheng Feng,Xiaohan Wu,Yaoyao Fan,Wei Zhang,Ming Ma,Ning Gu,Yu Zhang
Nanozymes with wide applications have rapidly attracted tremendous attention from various fields in the last decade. However, research on the standardization of nanozymes is still lacking. Currently, the accurate evaluation and effective tracing of the enzyme-like activity of nanozymes have become a common concern. This work aims to develop a certified reference material (CRM) of Prussian blue nanozymes (PBNEs) for their peroxidase (POD)-like activity. The homogeneity and stability studies demonstrated that the property value of POD-like activity is consistent across different packing units, and remains unchanged during the one-year validity period of storage in the dark at 4 °C. The certified value of the POD-like activity of the PBNE CRM is assigned as 174 ± 13 U mg−1 (k = 2) by interlaboratory comparison studies and traceable uncertain evaluation. Furthermore, the need for quality control of the POD-like activity of nanozymes was exemplified by comparing the influence of two additional PBNEs on the dry and wet chemical detection of glucose (Glu). As the first quality assurance tool of nanozymes, the PBNE CRM is expected to replace natural horse radish peroxidase (HRP) as an effective benchmark for assessing the analytical method and laboratory competence. In addition, this work also inspires the further standardization of nanozymes.
研究领域:
生物化学
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分析化学
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纳米医学
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DOI
PubMed
高影响因子
GEOSTANDARDS AND GEOANALYTICAL RESEARCH
·
2025
·
IF 3.4
Ai-qun Xiao,Pei-pei Zhao,Lu Yin,Bei Xu
A single-column extraction chromatographic purification method for tungsten using the N-benzoyl-N-phenylhydroxylamine (BPHA) resin was investigated in this study. This method greatly simplifies the W purification procedure, and only 10 ml of acid (5 ml 3 mol l -1 HCl-0.1 mol l -1 HF and 5 ml 1 mol l -1 HF) is required to separate W from Ti, Zr, Hf, Ta and other matrix elements. The blank in the separation step was less than 0.1 ng, and the recovery of W was ~ 99%. Six independent digestion measurements of reference materials BHVO-2, BCR-2, RGM-2 and JB-2 yielded μ 182 W values (mean value with intermediate precision, 95% confidence level) of -10.3 ± 4.0 ( n = 6, 2 s )，-1.2 ± 5.3 ( n = 6, 2 s )，-1.4 ± 4.4 ( n = 6, 2 s ) and 0.6 ± 3.8 ( n = 6, 2 s ), respectively, which are in good agreement with the previously reported values.
研究领域:
地球化学
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分析化学
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同位素地质学
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质谱分析
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DOI
高影响因子
Acta Geochimica
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2017
·Vol. 36
·期 3
·421-425
·
IF 0
Wu Guangliang,Zhu Jian-Ming,Tan Decan,Han Guilin,Zhang Lixing,Ren Kun
Lead (Pb) isotopes have been extensively employed in tracing sources of Pb and its transport pathways through the environment. However, Pb isotopic ratios in related geochemical reference materials are scarce. Here, we report high-precision Pb isotopic ratios measured by Nu Plasma II MC-ICP-MS using calibrated 205 Tl/ 203 Tl = 2.38865 (NIST SRM 997) for mass discrimination correction. The long-term external precision (2SD) for NIST SRM 981 of Pb, BCR-2, and BHVO-2 are 0.31‰ (n = 105), 0.42‰ (n = 11), and 0.25‰ (n = 5) for 208 Pb/ 206 Pb and 0.16‰, 0.53‰, and 0.07‰ for 206 Pb/ 207 Pb, both respectively, and their Pb isotopic ratios are in excellent agreement with the recommended values. Using this method, we report for the first time Pb isotopic compositions in shale SGR-1b (USGS); coal CLB-1 (USGS); stream sediments GSD-17, -21, and -23 (IGGE); soils GSS-12, -13, -14, -15, and -16 (IGGE); plants GSV-1, -2, and -3 (IGGE); and human hair GSH-1(IGGE).
研究领域:
地球化学
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环境科学
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产品关联
DOI
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
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2024
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IF 4
Xiaofang Li,Jinyan Li,Yongwei Feng,Liqiang Liu,Hua Kuang,Chuanlai Xu,Lingling Guo
Fumonisin Bs (FBs) are the most common toxic and carcinogenic substances found among naturally occurring contaminants of cereals. A group-specific monoclonal antibody (mAb) 2H7 was prepared that equably recognized fumonisins B 1 (FB 1 ), B 2 (FB 2 ), and B 3 (FB 3 ) with a half-maximal inhibitory concentration (IC 50 ) value for the three forms of 1.52, 2.93, and 3.85 ng/ml, respectively. On this basis, a fluorescent microsphere-based immunochromatographic strip (FM-ICS) was established for the rapid qualitative and quantitative detection of total FBs (FB 1 , FB 2 , and FB 3 ) in corn , wheat, and rice. A recovery test showed that the recovery of FM-ICS was 92.8–108.3% with coefficients of variation of 1.2–7.9%. This method has the same reliability as seen with liquid chromatography-tandem mass spectrometry. And the accuracy was further confirmed by certified reference materials. Therefore, it can be used for the detection of FBs in cereal samples.
研究领域:
食品科学
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分析化学
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毒理学
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DOI
高影响因子
TALANTA
·
2024
·
IF 5.6
Yongsheng Zhang,Jian Yuan,Rui Gao,Yang Zhao,Zefu Ye,Zhujun Zhu,Peihua Zhang,Lei Zhang,Wangbao Yin,Suotang Jia
Ash content, as a crucial indicator of coal quality, its rapid and accurate determination is pivotal to improve the energy utilization of coal and reduce environmental pollution. Traditional spectroscopic methods face significant challenges in acquiring accurate information from coal samples due to the notorious matrix effects arising from their complex composition, vast molecular structure, and diverse coal types. In this study, the feasibility of total reflection X-ray fluorescence (TXRF) combined with partial least squares (PLS) for the determination of coal ash was firstly investigated based on the TXRF being unaffected by matrix effects. Firstly, coal samples were prepared as suspensions, and the effects of sample particle size and different dispersants on the results of TXRF analyses were evaluated. The accuracy and applicability of the chosen sample preparation strategies were further validated using inductively coupled plasma mass spectrometry (ICP-MS) and two certified reference materials (CRMs). Subsequently, based on the analysis of 19 coal samples, the impact of three different predictive variables on the performance of the PLS model was investigated: (a) TXRF full spectrum normalized by the net intensity of the internal standard; (b) net intensity of characteristic peaks for 12 elements (Al, Si, K, Ca, Ti, Fe, Cr, Mn, Cu, Ni, and Sr) normalized by the net intensity of the internal standard; (c) concentrations of the aforementioned 12 elements. The results demonstrate that the PLS model constructed usingthe TXRF full spectrum normalized by the net intensity of the internal standard exhibits the best predictive capabilities, with the determination coefficient of calibration set (R 2 ) and mean square error (MSE) of the prediction set reaching 0.9736 and 0.99 %, respectively. Moreover, the measurement accuracy of this model was six times greater than that obtained with traditional X-ray fluorescence (XRF). Presented analytical results display the possibilities of combining TXRF with PLS for coal quality evaluation.
研究领域:
分析化学
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环境科学
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能源资源
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Xiaoyu Jia,Junyi Zhao,Hongyun Ren,Jiani Wang,Zixiao Hong,Xian Zhang
Zwitterion-functionalized polymer microspheres (ZPMs) have been designed and used as the core adsorbent for the selective and rapid enrichment of mercury species in environmental waters by an on-line solid-phase extraction (SPE). Zwitterionic S-ZPMs and N-ZPMs having an anionic sulfonic group, but differing in cationic S + and N + moieties were prepared from Merrifield resin by treating with 1,2-ethanedithiol and imidazole , followed by modification with 1,3-propanesultone. Without any additional reagents, inorganic mercury (In-Hg), methylmercury (MeHg) and ethylmercury (EtHg) were quantitatively adsorbed on the home-made mini-column packed with ZPMs. Following extraction with 60 mM ammonium acetate and 0.15% L -cysteine ( L -Cys) solution within seconds, separation and speciation of mercury were successfully achieved by the HPLC–ICP-MS technique. Under the optimized experimental conditions, the enrichment factors (EFs) are up to 105 and 98 for inorganic and organic mercury only with 40 mL sample solution, respectively. The low detection limits of 0.78 ng L −1 , 0.63 ng L −1 , and 0.49 ng L −1 were reached for In-Hg, MeHg and EtHg, respectively, with the relative standard deviations (RSDs) below 4.1%. The feasibility and accuracy of the on-line SPE–HPLC–ICP-MS method were successfully applied for mercury speciation in surface water, seawater as well as certified reference material (CRM). The results here demonstrate a facile, sensitive and selective method for speciation of mercury at trace levels.
研究领域:
分析化学
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环境科学
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化工工程
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产品关联
DOI
PubMed
高影响因子
MICROCHEMICAL JOURNAL
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2025
·
IF 5.1
Zhen-Wen Zhang,Ao-Jun Qiu,Geng-Jin-Sheng Cheng,Yu Fan,Yu Xiao,Yan-Zhu Liu,Qian-Yong Cao
Tetracycline detection remains an important research topic in the bioenvironmental field today. This paper reports a novel amphiphilic Eu(III) complex DO 3 AC 12 -Eu for single signal and ratiometric fluorescence detection of tetracycline (TC) in aqueous solution. DO 3 AC 12 -Eu can self-assemble micelle-like nano-aggregation in aqueous solution with no fluorescence. After addition of TC, the Eu(III)-based emission was observed for the effective antenna effect from TC to Eu(III) center. In addition, DO 3 AC 12 -Eu can load 4-methylumbelliferone sodium (MU) as a fluorescence reference to form DO 3 AC 12 -Eu/MU co-assembly nano-aggregation with a blue emission at 450 nm. Based on the TC-induced antenna effect and inner filter effect mechanism between TC and MU, DO 3 AC 12 -Eu/MU exhibits a ratiometrically fluorescent response toward TC, with increasing Eu(III)-based emission at 615 nm, and decreasing MU-based emission at 450 nm. Importantly, DO 3 AC 12 -Eu/MU exhibits superior sensitivity and selectivity over DO 3 AC 12 -Eu . The detection limit of DO 3 AC 12 -Eu/MU toward TC is 0.82 nM, far lower than that of DO 3 AC 12 -Eu (9.5 nM). Furthermore, DO 3 AC 12 -Eu/MU assembly has been successfully used for on-site and real-time detection of TC in food samples by using the smartphone-based visualization method and test gel.
研究领域:
分析化学
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环境监测
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生物环境科学
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荧光传感技术
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纳米科技
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配位化学
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食品安全检测
✓ 已验证
产品关联
DOI
高影响因子
TALANTA
·
2021
·
IF 6.057
Yunjia Yang,Man He,Beibei Chen,Bin Hu
A novel adsorbent of magnetic graphene oxide (GO) chemically modified by cysteamine hydrochloride (Fe 3 O 4 @SiO 2 /GO-NH 2 ) through thiol-ene click chemistry reaction was synthesized. The prepared Fe 3 O 4 @SiO 2 /GO-NH 2 exhibit selective adsorption to As(V) with high adsorption capacity (52.66 mg g −1 ). Taking Fe 3 O 4 @SiO 2 /GO-NH 2 as the adsorbents, a new method of magnetic solid phase extraction (MSPE) combined with graphite furnace atomic absorption spectrometry (GFAAS) was developed in determining trace-level inorganic arsenic species (As(III) and As(V)) in environmental water and bottled water samples. Various experimental parameters affecting the MSPE have been optimized. Under the optimal experimental parameters, the limit of detection of the established method for As(V) was 1.02 ng L −1 , the relative standard deviations were 7.9% (intra-day, c = 50 ng L −1 , n = 5) and 4.6% (inter-day, c = 50 ng L −1 , n = 7), respectively, and the enrichment factor of the method was 392. GBW08666 and GBW08667 (certified reference material) were analyzed to confirm the accuracy of the method, and the results were matched well with the certified values. The established MSPE-GFAAS method was successfully applied in analyzing trace/ultratrace As(III) and As(V) in real water samples.
研究领域:
环境化学
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分析化学
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材料科学
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2013
·
IF 3.498
Hong-mei Jiang,Ting Yang,Yan-hong Wang,Hong-zhen Lian,Xin Hu
A new approach of magnetic solid phase extraction (MSPE) coupled with graphite furnace atomic absorption spectrometry (GFAAS) has been developed for the speciation of Cr(III) and Cr(VI) using zincon-immobilized silica-coated magnetic Fe 3 O 4 nanoparticles (Zincon–Si–MNPs) as the MSPE absorbent. Cr(III) was quantitatively reserved on the absorbent at pH 9.1 while total Cr was reserved at pH 6.5. The absorbed Cr species were eluted by using 2 mol/L HCl and detected by GFAAS. The concentration of Cr(VI) could be calculated by subtracting Cr(III) from total Cr. All the parameters affecting the separation and extraction efficiency of Cr species such as pH, extraction time, concentration and volume of eluent , sample volume and influence of co-existing ions were systematically examined and the optimized conditions were established accordingly. The detection limit (LOD) of the method was 0.016 and 0.011 ng mL −1 for Cr(III) and Cr(VI), respectively, with the enrichment factor of 100 and 150. The precisions of this method (Relative standard deviation, RSD, n =7) for Cr(III) and Cr(VI) at 0.1 ng mL −1 were 6.0% and 6.2%, respectively. In order to validate the proposed method, a certified reference material of environmental water was analyzed, and the result of Cr speciation was in good agreement with the certified value. This MSPE–GFAAS method has been successfully applied for the speciation of Cr(III) and Cr(VI) in lake and tap waters with the recoveries of 88–109% for the spiked samples. Moreover, the MSPE separation mechanism of Cr(III) and Cr(VI) based on their adsorption–desorption on Zincon–Si–MNPs has been explained through various spectroscopic characterization.
研究领域:
分析化学
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环境科学
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材料科学
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产品关联
DOI
PubMed
高影响因子
TALANTA
·
2019
·
IF 4.916
Yi-Kun Li,Wei-tao Li,Xun Liu,Ting Yang,Ming-Li Chen,Jian-Hua Wang
A magnetic functionalized bio-sorbent based on aptamer was designed for the selective separation of ultra-trace Pb 2+ , shortly termed as Fe 3 O 4 @ [email protected] Pb(II) specific aptamer attached to the magnetic solid substrate served as affinity probe to capture and separate trace lead. Oligonucleotides with a polyA block were employed for the immobilization on the surface of AuNPs, with adenine sequences (polyA) as the part of effective anchoring block. The prepared Fe 3 O 4 @ [email protected] composites were characterized by FT-IR, SEM and XPS. The binding of lead on Fe 3 O 4 @ [email protected] composites surface was pH-dependent, the adsorption follows Langmuir model, and the adsorption dynamic fits the pseudo-second-order kinetics model. Procedure for lead separation and preconcentration was explored and combined with detection of graphite furnace atomic absorption spectrometry (GFAAS). Under the optimum condition, an enrichment factor of 17.73 was obtained with a sample volume of 1.0 mL. The limit of detection (LOD) was 57 ng L −1 along with a relative standard deviation (RSD) of 2.06 (n = 9). The procedure was further validated by a certified reference material GBW08608 and several environmental and blood samples.
研究领域:
环境科学
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分析化学
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材料科学
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生物化学
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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）