Analytical Chemistry Research最新文献_第2页

Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD) for the determination of PCBs in mussel samples 微基质固相色散法测定贻贝样品中多氯联苯的优化研究

Analytical Chemistry Research Pub Date : 2017-03-01 DOI: 10.1016/j.ancr.2016.11.003

Nieves Carro, Laura Vilas, Isabel García, María Ignacio, Ana M. Mouteira

{"title":"Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD) for the determination of PCBs in mussel samples","authors":"Nieves Carro, Laura Vilas, Isabel García, María Ignacio, Ana M. Mouteira","doi":"10.1016/j.ancr.2016.11.003","DOIUrl":"10.1016/j.ancr.2016.11.003","url":null,"abstract":"<div><p>This paper reports the development and optimization of micro-matrix solid-phase dispersion (micro-MSPD) of nine polychlorinated biphenyls (PCBs) in mussel samples (<em>Mytilus galloprovincialis</em>) by using a two-level factorial design. Four variables (amount of sample, anhydrous sodium sulphate, Florisil and solvent volume) were considered as factors in the optimization process. The results suggested that only the interaction between the amount of anhydrous sodium sulphate and the solvent volume was statistically significant for the overall recovery of a trichlorinated compound, CB 28. Generally most of the considered species exhibited a similar behaviour, the sample and Florisil amounts had a positive effect on PCBs extractions and solvent volume and sulphate amount had a negative effect. The analytical determination and confirmation of PCBs were carried out by using GC-ECD and GC-MS/MS, respectively. The method was validated having satisfactory precision and accuracy with RSD values below 6% and recoveries between 81 and 116% for all congeners. The optimized method was applied to the extraction of real mussel samples from two Galician Rías.</p></div>","PeriodicalId":7819,"journal":{"name":"Analytical Chemistry Research","volume":"11 ","pages":"Pages 1-8"},"PeriodicalIF":0.0,"publicationDate":"2017-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ancr.2016.11.003","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90673220","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 12

Enhancement of the atomic absorbance of Cr, Zn, Cd, and Pb in metal furnace atomic absorption spectrometry using absorption tubes 利用吸收管增强金属炉原子吸收光谱法中Cr、Zn、Cd和Pb的原子吸收

Analytical Chemistry Research Pub Date : 2017-03-01 DOI: 10.1016/j.ancr.2016.11.004

Yuya Koike , Kenta Hagiwara , Toshihiro Nakamura

引用次数: 8

Cloud point assisted dispersive ionic liquid -liquid microextraction for chromium speciation in human blood samples based on isopropyl 2-[(isopropoxycarbothiolyl)disulfanyl] ethane thioate 云点辅助分散离子液体-基于异丙基2-[(异丙氧基碳硫基)二磺胺基]乙烷硫酸盐的人体血液样品中铬形态的液体微萃取

Analytical Chemistry Research Pub Date : 2016-12-01 DOI: 10.1016/j.ancr.2016.10.002

Hamid Shirkhanloo , Mehri Ghazaghi , Mohammad Mehdi Eskandari

{"title":"Cloud point assisted dispersive ionic liquid -liquid microextraction for chromium speciation in human blood samples based on isopropyl 2-[(isopropoxycarbothiolyl)disulfanyl] ethane thioate","authors":"Hamid Shirkhanloo , Mehri Ghazaghi , Mohammad Mehdi Eskandari","doi":"10.1016/j.ancr.2016.10.002","DOIUrl":"10.1016/j.ancr.2016.10.002","url":null,"abstract":"<div><p>An efficient and fast method based on isopropyl 2-[(isopropoxycarbothiolyl)disulfanyl] ethane thioate (IICDET) were used for the speciation and determination of trace amount of Cr(III and VI) in human biological samples by cloud point assisted dispersive ionic liquid –liquid microextraction (CP-DILLME). Cr(VI) has carcinogenic effects, so, speciation of chromium in human body such as blood cells is very important. The cloudy solution was achieved by the mixture of acetone and IL ([C<sub>8</sub>MIM][PF<sub>6</sub>]) in human blood samples containing Cr(III) ions that were already complexed by IICDET at pH 4.5. After reduction Cr(VI) to Cr(III) by ascorbic acid, chromium speciation was obtained based on total chromium determination by electro thermal atomic absorption spectrometry (ET-AAS) and difference between total Cr and Cr(III) content. In addition, Cr speciation in human blood cells was calculated based on IICDET/CP-DILLME and hematocrit blood test (HCT). After optimized conditions, the enrichment factor (EF), Linear range and limit of detection (LOD) was obtained 25.2, 0.02–1.75 μg L<sup>−1</sup> and 5.4 ng L<sup>−1</sup> in human biological samples respectively. The validation of methodology was achieved by certified reference material (CRM) and ICP-MS technique.</p></div>","PeriodicalId":7819,"journal":{"name":"Analytical Chemistry Research","volume":"10 ","pages":"Pages 18-27"},"PeriodicalIF":0.0,"publicationDate":"2016-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ancr.2016.10.002","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77164601","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 27

Towards coupling dispersive liquid-liquid microextraction with hollow fibre liquid phase microextraction for extraction of organic pollutants of agricultural origin 分散液液微萃取与中空纤维液相微萃取耦合萃取农业有机污染物的研究

Analytical Chemistry Research Pub Date : 2016-12-01 DOI: 10.1016/j.ancr.2016.11.001

Thabiso Letseka, Mosotho J. George

{"title":"Towards coupling dispersive liquid-liquid microextraction with hollow fibre liquid phase microextraction for extraction of organic pollutants of agricultural origin","authors":"Thabiso Letseka, Mosotho J. George","doi":"10.1016/j.ancr.2016.11.001","DOIUrl":"10.1016/j.ancr.2016.11.001","url":null,"abstract":"<div><p>Liquid-based miniaturized techniques have received a lot of attention recently resulting in the development of the liquid phase microextraction (LPME) and dispersive liquid-liquid microextraction (DLLME) techniques each offering unique benefits over the other technique. Herein we report a combination of the two techniques for the extraction of hexestrol and atrazine from aqueous systems. The method sets off with the DLLME thereafter a hollow fibre filled with the organic solvent is introduced for the extraction of the pre-extracted analytes in the dispersed organic solvent. The method was modified further by introducing a second extracting solvent in place of the disperser solvent. Under the optimum conditions, namely, toluene in the acceptor phase, 1:1 chloroform:toluene (v/v) as a dispersed solvent, 15% NaCl, with the 15 min extraction time, the method achieved satisfactory enrichment factors (87- and 62-fold); sufficiently low detection limits of 0.018 μg/mL and 0.016 μg/mL using the flame ionization detector, while 0.072 and 0.063 ng/mL were obtained using single ion monitoring mass spectrometry detector, for atrazine and hexestrol, respectively; with sufficient linearity (R<sup>2</sup> ≥ 0.9959). Although the compounds were not detected in the river water sample, satisfactory recoveries (111–115%) were achieved indicating the method did not suffer any negative matrix effect.</p></div>","PeriodicalId":7819,"journal":{"name":"Analytical Chemistry Research","volume":"10 ","pages":"Pages 28-32"},"PeriodicalIF":0.0,"publicationDate":"2016-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ancr.2016.11.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79137346","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 17

Spectrophotometric determination of ammonia nitrogen in water by flow injection analysis based on NH3- o-phthalaldehyde -Na2SO3 reaction NH3-邻苯二醛- na2so3反应流动注射分光光度法测定水中氨氮

Analytical Chemistry Research Pub Date : 2016-12-01 DOI: 10.1016/j.ancr.2016.10.001

Ying Liang, Chunmei Yan, Qing Guo, Jin Xu, Hongzhi Hu

{"title":"Spectrophotometric determination of ammonia nitrogen in water by flow injection analysis based on NH3- o-phthalaldehyde -Na2SO3 reaction","authors":"Ying Liang, Chunmei Yan, Qing Guo, Jin Xu, Hongzhi Hu","doi":"10.1016/j.ancr.2016.10.001","DOIUrl":"10.1016/j.ancr.2016.10.001","url":null,"abstract":"<div><p>The product of the NH<sub>3</sub>- <em>o-</em>phthalaldehyde (OPA) -Na<sub>2</sub>SO<sub>3</sub> reaction is rose red at pH more than 10.4, and its maximum absorption wavelength is 550 nm. Based on this, a novel spectrophotometric method with flow injection analysis has been established to determine ammonia nitrogen in water. Experimental parameters related to the flow injection method and the reaction were optimized throughout the experiments based on univariate experimental design. The length of coil is optimized as 1.6 m for storing up standard or sample solution. The optimal value is 8.20 mL/min for loading flow rate of coloring solution. The OPA concentration, sulfite concentration and reaction pH are chosen as 1.06 g/L, 0.050 g/L and 10.80, respectively. The reaction temperature and stop flow time affects the performances of the method. The linearity range and detection limit of the proposed method are 0.100–0.700 mmol/L and 0.007 mmol/L at the reaction temperature of 55 °C and stop flow time of 340 s, respectively. The sample throughput is more than 8 h<sup>−1</sup>. Under the optimal experimental conditions, the recovery is 100.4%, 95.2%, 101.7% and 92.4% for the lake water, river water, groundwater and sewage, respectively. Two lake water samples were analyzed using both the proposed method and indophenol blue method, the results show no significant difference between these two methods. In comparison with other spectrophotometric determination method of ammonia nitrogen, the main merits of the proposed method are simplicity, reliability, reproducibility and high sample throughput.</p></div>","PeriodicalId":7819,"journal":{"name":"Analytical Chemistry Research","volume":"10 ","pages":"Pages 1-8"},"PeriodicalIF":0.0,"publicationDate":"2016-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ancr.2016.10.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73998316","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 39

Double-functionalized magnetic nanoparticles for preconcentration and determination of polycyclic aromatic hydrocarbons in water samples 用于水样中多环芳烃预富集和测定的双功能化磁性纳米颗粒

Analytical Chemistry Research Pub Date : 2016-12-01 DOI: 10.1016/j.ancr.2016.10.003

A.A. Al-rashdi

引用次数: 19

Extraction and recovery of 2-butoxyethanol from aqueous phases containing high saline concentration 高盐水溶液中2-丁氧基乙醇的提取和回收

Analytical Chemistry Research Pub Date : 2016-09-01 DOI: 10.1016/j.ancr.2016.07.001

Katherine E. Manz , Kimberly E. Carter

{"title":"Extraction and recovery of 2-butoxyethanol from aqueous phases containing high saline concentration","authors":"Katherine E. Manz , Kimberly E. Carter","doi":"10.1016/j.ancr.2016.07.001","DOIUrl":"10.1016/j.ancr.2016.07.001","url":null,"abstract":"<div><p>Ethylene glycol monobutyl ether (EGBE), also known as 2-butoxyethanol (2-BE), has been identified as a contaminant in hydraulic fracturing fluids. In order to determine the presence of 2-BE in hydraulic fracturing chemical additives, a reliable method for recovering 2-BE from aqueous phases by liquid-liquid extraction combined with gas chromatography/mass spectrometry (GC/MS) was established. The liquid-liquid extraction method was applied to samples matrices containing various amounts of salt. Using methylene chloride for liquid-liquid extraction in a sample to solvent ratio of 1:3, ≥99% 2-BE recovery may be achieved with less than 5% standard error. The limit of detection was determined to be 0.957 mg L<sup>−1</sup> 2-BE. Accuracy was determined to be 2.58% and precision was determined using the coefficient of variation, which was 3.5%. The method was used to recover 2-BE in a hydraulic fracturing chemical additive called Revert Flow and to quantify the weight percent of 2-BE in the chemical additive. Weight percent of two additional components of Revert Flow, D-limonene and 1-butoxy-2-propanol, were also determined. We also used the method to determine the abiotic of 2-BE in water, which was 5.55 days. The persistence of 2-BE in hydraulic fracturing fluid was also investigated and determined that 2-BE is more persistent in this environment.</p></div>","PeriodicalId":7819,"journal":{"name":"Analytical Chemistry Research","volume":"9 ","pages":"Pages 1-7"},"PeriodicalIF":0.0,"publicationDate":"2016-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ancr.2016.07.001","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82432949","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 9

Quantification of 3α-hydroxytibolone in human plasma by high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS): Application in a bioequivalence study in healthy postmenopausal volunteers 高效液相色谱-电喷雾电离串联质谱法(HPLC-ESI-MS/MS)定量测定人血浆中3α-羟基替布洛酮:在健康绝经后志愿者生物等效性研究中的应用

Analytical Chemistry Research Pub Date : 2016-06-01 DOI: 10.1016/J.ANCR.2016.04.002

Lucas Azevedo Portela, T. L. Laurito, B. Severino, E. Perissutti, G. Mendes, R. Moreno, G. Nucci

引用次数: 3

Quantification of 3α-hydroxytibolone in human plasma by high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS): Application in a bioequivalence study in healthy postmenopausal volunteers 高效液相色谱-电喷雾电离串联质谱法(HPLC-ESI-MS/MS)定量测定人血浆中3α-羟基替布洛酮:在健康绝经后志愿者生物等效性研究中的应用

Analytical Chemistry Research Pub Date : 2016-06-01 DOI: 10.1016/j.ancr.2016.04.002

Lucas Azevedo Portela , Tiago Luders Laurito , Beatrice Severino , Elisa Perissutti , Gustavo D. Mendes , Ronilson Agnaldo Moreno , Gilberto De Nucci

{"title":"Quantification of 3α-hydroxytibolone in human plasma by high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS): Application in a bioequivalence study in healthy postmenopausal volunteers","authors":"Lucas Azevedo Portela , Tiago Luders Laurito , Beatrice Severino , Elisa Perissutti , Gustavo D. Mendes , Ronilson Agnaldo Moreno , Gilberto De Nucci","doi":"10.1016/j.ancr.2016.04.002","DOIUrl":"https://doi.org/10.1016/j.ancr.2016.04.002","url":null,"abstract":"<div><p>A sensitive, specific and fast method to quantify 3α-hydroxytibolone in human plasma using deuterated 3α-hydroxytibolone (d5) as internal standard is described. The analyte and the internal standard were extracted from plasma (900 μL) by liquid-liquid extraction using ethyl ether/hexane (50/50, v/v) and ammonium hydroxide (50%). The extracts were analyzed by high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry without derivatization. Chromatography was performed isocratically on a Gemini-NX™ C<sub>18</sub> 5 μm (150 × 4.6 mm i. d.) column. The method had a chromatographic run time of 3.75 min and a linear calibration curve over the range 1–100 ng/mL. The limit of quantification validated was 1 ng/mL. This method was used to assess the bioequivalence between two different tibolone oral formulations: Livolon (1.25 mg tablet) provided by Biolab Sanus Farmacêutica (Brazil), as the test formulation, and Libiam™ (1.25 mg tablet) produced by Libbs Farmacêutica (Brazil), as the reference formulation. A single 3.75 mg dose of each formulation was administered to 46 postmenopausal female healthy volunteers. The study was conducted in an open, randomized, two-period crossover balanced design with a 2 week washout interval between the doses. The 90% confidence interval for C<sub>max</sub>, AUC<sub>(0-last)</sub> and AUC<sub>(0-inf)</sub> individual test/reference ratios were 97.48–111.51, 95.35–103.20 and 96.42–103.86, respectively. It is concluded that Livolon (1.25 mg tablet) is bioequivalent to Libiam™ (1.25 mg tablet), with regards to both rate and extent of absorption.</p></div>","PeriodicalId":7819,"journal":{"name":"Analytical Chemistry Research","volume":"8 ","pages":"Pages 16-25"},"PeriodicalIF":0.0,"publicationDate":"2016-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/j.ancr.2016.04.002","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90017782","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 3

Chromogenic signaling of water traces by 1,8-naphthalohydrazone-anion complex in organic solvents 1,8-萘酰腙阴离子络合物在有机溶剂中水迹的显色信号

Analytical Chemistry Research Pub Date : 2016-06-01 DOI: 10.1016/j.ancr.2016.03.001

Veikko Uahengo , Bi Xiong , Ping Cai , Likius S. Daniel , Lydia Rhyman , Ponnadurai Ramasami

引用次数: 4