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Determination of ethanol in blood using headspace gas chromatography with flameionization detector (HS-GC-FID): Validation of a method 顶空气相色谱-火焰化检测器(HS-GC-FID)测定血液中乙醇的方法验证
Pub Date : 2020-01-01 DOI: 10.1080/23312009.2020.1760187
L. D. Mihretu, Asfaw Gebretsadik Gebru, K. Mekonnen, Abraha Gebrekidan Asgedom, Ykalo Hadush Desta
Abstract Ethanol is a common psychoactive substance that has been widely consumed in several parts of the world. Gas chromatography (GC) coupled with flame ionisation detector (FID) has often been used for the determination of blood alcohol concentration. The aim of this study was to develop and validate a very simple and reliable HS-GC-FID method for quantitative determination of ethanol in blood sample. Validation of the method was performed by means of Bias, Linearity, LOD, Selectivity, Specificity, Precision, Robustness and Intermediate precision. The method showed an excellent linearity with correlation coefficient (r2 = 0.993) was observed in the range from 0.1 to 3.5 mg/mL of ethanol. The percent recovery value were between 91.0 and 109.1 which was with an acceptable percent recovery, The precision (repeatability) was reported as 27 % and intermediate precision of the method resulted in 11% and 1 % for two analysts. The limit of detection (LOD) of ethanol was calculated as 0.099 mg/mL and the selectivity of the method for interferents (methanol and acetaldehyde) was totally selective. Generally, the results obtained confirmed that the method is relatively fast, precise, simple, robust and can be used in routine forensic analyses for the determination of blood alcohol concentration (BAC) at a concentration level greater than 0.13 mg/mL.
摘要乙醇是一种常见的精神活性物质,在世界各地被广泛消费。气相色谱法(GC)和火焰离子化检测器(FID)经常用于测定血液中的酒精浓度。本研究的目的是开发和验证一种非常简单可靠的HS-GC-FID方法来定量测定血液样品中的乙醇。通过偏倚、线性、LOD、选择性、特异性、精密度、稳健性和中间精密度对该方法进行验证。该方法显示出良好的线性,在0.1至3.5mg/mL的乙醇范围内观察到相关系数(r2=0.993)。回收率在91.0和109.1之间,回收率在可接受的范围内。精密度(重复性)报告为27%,两名分析员的方法中间精密度分别为11%和1%。乙醇的检测限(LOD)计算为0.099mg/mL,该方法对干扰物质(甲醇和乙醛)的选择性是完全选择性的。通常,所获得的结果证实,该方法相对快速、准确、简单、稳健,可用于常规法医分析,以确定浓度水平大于0.13mg/mL的血液酒精浓度(BAC)。
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引用次数: 9
Statistical analysis of trace metals content of cocaine using inductively coupled plasma-mass spectrometry calibrations 电感耦合等离子体质谱法校正可卡因痕量金属含量的统计分析
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1671071
Edward Bentil, N. Asiedu, James Ataki
Abstract The trafficking of cocaine has become a global challenge now and Ghana is no exception. Cocaine is a whitish powder, which is, produced both from natural and synthetic means. This paper studied the metal content of seized cocaine in Ghana and the data used for batch identification. Ten metals, namely, Pb, Cu, Mg, Mn, Cr, As, Ni, Fe, Co and Ca were analyzed in 37 samples which were sampled from 2010 to 2014. Analyses of the metals were done using ICP-MS and data was analyzed using statistical tools. The results showed that, calcium recorded the highest amount in all the samples with a mean of 64.94mg/kg followed by Magnesium, Zinc and Iron with mean values of 24.35mg/kg, 6.25mg/kg and 2.65mg/kg, respectively. All the samples, within-seizure classification under class A showed to significant differences between each pair at a confidence level of 95%. With three sample pairs under class B in the within-seizure classification, one of the pairs; 103A and 105B showed no significant differences between them even though they were sampled from two different packages from the same seizure. Five samples from five different seizures also showed a significant difference among them showing that they came from different batches or origin. It is confirmed that seized cocaine contained poisonous heavy metals like Lead, Arsenic and Chromium, which have the amount that could affect the user-provide figures. Based on the data gathered from the within-seizure class A group, it could be proposed that a missing cocaine could be identified by its metal content.
摘要可卡因贩运已成为一项全球性挑战,加纳也不例外。可卡因是一种白色粉末,由天然和合成两种方法生产。本文研究了加纳缉获的可卡因中的金属含量以及用于批量鉴定的数据。对2010年至2014年采样的37个样品中的Pb、Cu、Mg、Mn、Cr、As、Ni、Fe、Co和Ca等10种金属进行了分析。使用ICP-MS对金属进行分析,并使用统计工具对数据进行分析。结果表明,所有样品中钙含量最高,平均为64.94mg/kg,其次是镁、锌和铁,平均值分别为24.35mg/kg、6.25mg/kg和2.65mg/kg。在A类癫痫发作分类范围内的所有样本显示,每对样本之间存在显著差异,置信水平为95%。在癫痫发作内分类中,B类下有三对样本,其中一对;103A和105B显示它们之间没有显著差异,即使它们是从同一次缉获的两个不同包裹中取样的。来自五次不同癫痫发作的五份样本也显示出它们之间的显著差异,表明它们来自不同的批次或来源。经证实,缉获的可卡因含有铅、砷和铬等有毒重金属,其含量可能会影响使用者提供的数据。根据从缉获内A类组收集的数据,可以提出,可以通过其金属含量来识别失踪的可卡因。
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引用次数: 2
Calibration development for nutritional evaluation of Yam (Dioscorea sp.) using Near-Infrared Reflectance Spectrophotometry (NIRS) 近红外反射分光光度法用于薯蓣营养评价的标定方法研究
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1565623
O. E. Alamu, M. Adesokan, B. Maziya-Dixon
Abstract The aim of yam breeders is to produce many hybrids, which can form the basis of selecting quality nutritional traits and other characteristics using certain agronomic criteria. Chemical methods are employed to determine the main constituents of yam, which are time-consuming, expensive, and involve sample destruction. However, the constraints of lengthy analysis time and the cost needed to analyze thousands of these genotypes are major constraints to yam breeding in Nigeria. This study was undertaken to develop and validate calibration equations on the Near-Infrared Reflectance Spectrophotometer (NIRS) for determining chemical compositions of selected yam genotypes. Equations developed for moisture, ash, protein, crude fiber, and tannin showed high coefficients of determination (R2) for the calibration curve (0.87, 0.84, 0.83, 0.80, and 0.89, respectively) and high to medium coefficients of determination in cross-validation (0.80, 0.68, 0.69, 0.68, and 0.50). The standard errors of calibration (SEC) and the standard errors in cross-validation (SECV) were low for most constituents. A total of 360 ascensions of yam flour were predicted for selected traits to test the equations, and the results were comparable with data from conventional methods. Results of this study have shown that NIRS could be a very useful tool to help yam breeders screen large sample sets using limited resources with very short time. This will enhance breeders’ rapid selection of genotypes at screening stage where many breeding lines are to be evaluated within the shortest time possible.
摘要育种家的目标是培育出许多杂交种,这些杂交种可以利用某些农艺标准为选择优质营养性状和其他特性奠定基础。采用化学方法测定yam的主要成分,耗时、昂贵,并涉及样品销毁。然而,分析时间长和分析数千种此类基因型所需的成本是尼日利亚山药育种的主要制约因素。本研究旨在开发和验证近红外反射分光光度计(NIRS)上的校准方程,以确定选定的yam基因型的化学成分。为水分、灰分、蛋白质、粗纤维、,和单宁在校准曲线上显示出较高的测定系数(R2)(分别为0.87、0.84、0.83、0.80和0.89),在交叉验证中显示出较高至中等的测定系数。大多数成分的校准标准误差(SEC)和交叉验证标准误差(SECV)较低。通过对所选性状的分析,预测了甘薯粉的360次上升,并对方程进行了检验,结果与传统方法的数据相比较。这项研究的结果表明,NIRS可能是一个非常有用的工具,可以帮助山药育种家在很短的时间内利用有限的资源筛选大样本集。这将增强育种家在筛选阶段对基因型的快速选择,在筛选阶段,许多育种系将在尽可能短的时间内进行评估。
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引用次数: 10
A comparison of the transition metal concentrations in the faeces, urine, and manure slurry from different livestock animals related to environmentally relevant microbial processes 与环境相关的微生物过程有关的不同家畜的粪便、尿液和粪肥浆中过渡金属浓度的比较
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1644702
S. Svane, H. Karring
Abstract The microbiological communities in livestock manure slurries produce gases of environmental concern such as ammonia, methane and nitrous oxide and require trace metals such as nickel, iron, and copper to synthesize active metalloenzymes that catalyse key biochemical reactions. Additionally, large quantities of trace metals are supplied to the soil when animal manure/manure slurry is used as a fertilizer, which has led to more strict legislation regarding metal contents in manure slurry. In this study, the concentrations of the environmentally relevant transition metals nickel (Ni), copper (Cu), zinc (Zn), iron (Fe), and manganese (Mn) in faeces and urine from pigs, cattle and horses were determined using graphite furnace and flame atomic absorption spectroscopy. We show that for all three animal species 97–100% of the metal contents in manure slurry originate from faeces. The analyses show that uncontaminated manure slurry from pigs has higher metal contents than the manure slurries from cattle and horses. Specifically, on a dry matter (dm) basis, pig manure slurry contains approximately 8 mg Ni/kg dm, 104 mg Cu/kg dm, 185 mg Zn/kg dm, 1134 mg Fe/kg dm, and 356 mg Mn/kg dm. Comparing the determined transition metal contents with published values for manure/manure slurry reveals that especially Cu, Zn and Fe concentrations in manure slurry have decreased in recent years. Comparing our results with other observations suggest that the levels of Ni, Cu, Zn, Fe, and Mn in manure slurries do not limit the microbial processes involved in the production or assimilation of environmentally relevant biogenic gasses.
摘要牲畜粪便浆中的微生物群落产生氨、甲烷和一氧化二氮等环境问题气体,并需要镍、铁和铜等微量金属来合成催化关键生物化学反应的活性金属酶。此外,当使用动物粪便/粪肥浆作为肥料时,会向土壤中供应大量微量金属,这导致了对粪肥浆中金属含量的更严格立法。在本研究中,使用石墨炉和火焰原子吸收光谱法测定了猪、牛和马粪便和尿液中与环境相关的过渡金属镍(Ni)、铜(Cu)、锌(Zn)、铁(Fe)和锰(Mn)的浓度。我们发现,对于所有三种动物,粪肥浆中97–100%的金属含量来自粪便。分析表明,未受污染的猪粪浆的金属含量高于牛马粪浆。具体而言,在干物质(dm)的基础上,猪粪浆含有约8 mg Ni/kg dm、104 mg Cu/kg dm、185 mg Zn/kg dm、1134 mg Fe/kg dm和356 mg Mn/kg dm。将测定的过渡金属含量与粪肥/粪肥浆的公布值进行比较表明,近年来粪肥浆中的Cu、Zn和Fe浓度尤其有所下降。将我们的结果与其他观察结果进行比较表明,粪肥浆中Ni、Cu、Zn、Fe和Mn的水平并没有限制与环境相关的生物气体的产生或同化所涉及的微生物过程。
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引用次数: 11
Voltammetric determination of paracetamol in pharmaceutical tablet samples using anthraquinone modified carbon paste electrode 蒽醌修饰碳糊电极伏安法测定片剂中扑热息痛的含量
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1576349
Meareg Amare, Welday Teklay
Abstract After cyclic voltammetric investigation of the electrochemical behavior of paracetamol and dependence of peak current on scan rate and pH; square wave voltammetric method based on anthraquinone modified carbon paste electrode was developed for direct determination of paracetamol in pharmaceutical tablet samples. In contrast to the peak potential at the unmodified electrode, appearance of the oxidative peak at a lower potential at the modified electrode indicated a catalytic property of the modifier towards paracetamol oxidation. While the observed peak potential shift with scan rate confirmed the irreversibility of the reaction, comparable correlation coefficients for the dependence of peak current of scan rate and square root of scan rate indicated that the irreversible oxidation reaction was controlled by both diffusion and adsorption. The peak current response of the developed method showed a linear dependence on the paracetamol concentration in the range 5 to 150 ppm. Excellent recoveries (93.5%), wide dynamic range, low limit of detection (0.13 µM), and limit of quantification (0.43 µM) validated the method for determination of paracetamol in real samples. The proposed method was applied for paracetamol determination in four brands of tablet samples (Julphare Aldol, Panadol Adva, Kelvin, and Para Denk) all of which labeled 500 mg/tablet. The paracetamol content of the analyzed four brands of tablet samples using the reported method was ranged between 83.04% (Panadol Adva, Kenya) and 95.08% (Para Denk, Germany) of the labeled amount. The discrepancy might be ascribed to the possible matrix difference among the companies and/or failure of the companies to comply the standard.
循环伏安法研究了对乙酰氨基酚的电化学行为及峰值电流与扫描速率和pH的关系;建立了基于蒽醌修饰碳糊电极的方波伏安法直接测定片剂中扑热息痛的含量。与未修饰电极上的峰电位相比,修饰电极上较低电位下氧化峰的出现表明改性剂对扑热息痛氧化具有催化性能。峰电位随扫描速率的变化证实了反应的不可逆性,而峰值电流随扫描速率的变化与扫描速率的平方根的相关性表明,不可逆性氧化反应同时受到扩散和吸附的控制。该方法的峰值电流响应与对乙酰氨基酚浓度在5 ~ 150ppm范围内呈线性关系。该方法回收率高(93.5%),动态范围宽,检出限低(0.13µM),定量限低(0.43µM),可用于实际样品中扑热息痛的测定。应用该方法测定了标签为500 mg/片的4个品牌(Julphare Aldol、Panadol Adva、Kelvin和Para Denk)对乙酰氨基酚的含量。采用该方法分析的4个品牌片剂样品的扑热息痛含量范围为标签量的83.04% (Panadol Adva,肯尼亚)~ 95.08% (Para Denk,德国)。这种差异可能归因于公司之间可能存在的矩阵差异和/或公司未能遵守标准。
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引用次数: 19
Palladium-catalyzed amination of 2-chlorothienopyridone with primary aromatic amines 钯催化2-氯噻吩并吡啶酮与伯芳香胺的胺化反应
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1567894
Samir A. Al-taweel, Salah A Al-Trawneh, Wal'A M. Al-Trawneh
Abstract A series of ethyl 7-cyclopropyl-2-(arylamino)-3-nitro-4-oxo-4,7-dihydrothieno[2,3-b]pyridine-5-carboxylate (9a-d) were prepared by coupling of ethyl 7-cyclopropyl-2-chloro-3-nitro-4-oxo-4,7-dihydrothieno[2,3-b]pyridine-5-carboxylate (8) with primary aromatic amines via palladium-catalyzed amination using palladium acetate Pd(OAc)2 in the presence of cesium fluoride in good yields. The new compounds were characterized by 1H-NMR, 13C-NMR, mass spectrometry, high resolution mass spectrometry and elemental analysis. 7-cyclopropyl-2-(phenylamino)-3-nitro-4-oxo-4,7-dihydrothieno[2,3-b]pyridine-5-carboxylic acid (10a) showed weak activity against E.aerogenas and S.aureus bacteria.
摘要在氟化铯存在下,采用钯催化醋酸钯Pd(OAc)2,将7-环丙基-2-(芳基氨基)-3-硝基-4-氧-4,7-二氢噻吩[2,3-b]吡啶-5-羧酸酯(8)与伯胺偶联,制备了一系列7-环丙基-2-(芳基氨基)-3-硝基-4-氧-4,7-二氢噻吩[2,3-b]吡啶-5-羧酸酯(9a-d)。通过1H-NMR、13C-NMR、质谱、高分辨率质谱和元素分析对化合物进行了表征。7-环丙基-2-(苯胺)-3-硝基-4-氧-4,7-二氢噻吩[2,3-b]吡啶-5-羧酸(10a)对e .气原菌和金黄色葡萄球菌的活性较弱。
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引用次数: 1
AmberliteTM IRA67: A novel and efficient ion exchange resin catalyst for the synthesis of 1, 8-dioxoxanthene derivatives AmberliteTM IRA67:一种新型高效离子交换树脂催化剂,用于合成1,8-二氧杂蒽衍生物
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1708160
N. Babu G., W. Belay, Teju Endale
Abstract The catalytic performance of AmberliteTM IRA67, the heterogeneous weak Base Exchange resin which bears tertiary amine functional group, for the synthesis of 1, 8-dioxoxanthene derivatives were investigated. The AmberliteTM IRA67 heterogeneous resin catalyst was found to be efficient and easily recoverable in the reaction of aromatic aldehydes and 5,5-dimethyl-1,3-cyclohexanedione to their corresponding 1, 8-dioxoxanthene derivatives under novel reaction conditions. Short reaction times, excellent yields (88–98%) and simple experimental procedure with an easy work-up are some of the advantages of the procedure. A total of 11 new compounds have been synthesized with a variety of substituent. The characterization of the compounds was completed using melting point determination, FT-IR, 1H-NMR, and 13C-NMR spectroscopic methods. The AmberliteTM IRA67 catalyst could be easily recovered after reaction completion and reused six times with an excellent durability and without any noticeable loss in activity. Furthermore, this general and simple method may be of much significance in many of other catalytic applications. Graphical Abstract
摘要研究了带有叔胺官能团的非均相弱碱交换树脂AmberliteTM IRA67对合成1,8-二氧杂蒽衍生物的催化性能。AmberliteTM IRA67多相树脂催化剂被发现在新的反应条件下,在芳香醛和5,5-二甲基-1,3-环己烷二酮与它们相应的1,8-二氧杂蒽衍生物的反应中是有效的并且容易回收。反应时间短,产率高(88–98%),实验过程简单,后处理容易,是该方法的一些优点。共合成了11个具有各种取代基的新化合物。使用熔点测定、FT-IR、1H-NMR和13C-NMR光谱方法完成了化合物的表征。AmberliteTM IRA67催化剂在反应完成后可以很容易地回收并重复使用六次,具有优异的耐久性且没有任何明显的活性损失。此外,这种通用而简单的方法在许多其他催化应用中可能具有重要意义。图形摘要
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引用次数: 4
Electrochemical determination of paracetamol, rutin and sulfonamide in pharmaceutical formulations by using glassy carbon electrode – A Review 玻璃碳电极电化学测定药物制剂中扑热息痛、芦丁和磺胺的研究进展
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1681607
A. Kassa, Meareg Amare
Abstract Recent advances in the electrochemical application of glassy carbon electrode for determination of selected drugs in pharmaceutical formulations are reviewed. Several analytical techniques such as liquid chromatography, high performance liquid chromatography, spectrophotometry, chemiluminescence, and capillary electrophoresis-mass spectrometry have been used for the detection and separation of pharmaceutical active components due to their high sensitivity and great selectivity. However, all these methods are complicated, time-consuming and require expensive equipment. In contrast to these conventional techniques, the electrochemical technique overcomes those drawbacks owing to its low cost, rapid response and application in on-site test. Special attention is paid on this review for electrochemical application of bare and modified glassy carbon electrode for the determination of paracetamol, rutin and sulfonamide in pharmaceutical formulation.
摘要综述了玻碳电极在药物制剂中选择性药物测定中的电化学应用的最新进展。几种分析技术,如液相色谱法、高效液相色谱、分光光度法、化学发光法和毛细管电泳质谱法,由于其高灵敏度和高选择性,已被用于药物活性成分的检测和分离。然而,所有这些方法都是复杂的、耗时的并且需要昂贵的设备。与这些传统技术相比,电化学技术由于其低成本、快速响应和在现场测试中的应用而克服了这些缺点。综述了裸玻碳电极和修饰玻碳电极在药物制剂中对乙酰氨基酚、芦丁和磺酰胺含量测定中的电化学应用。
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引用次数: 12
Modelling the distribution of arsenic and mercury in urine using chemometric tools 利用化学计量工具模拟尿液中砷和汞的分布
Pub Date : 2019-01-01 DOI: 10.1080/23312009.2019.1586064
Bernard Adu-Poku, N. Asiedu, O. Akoto, James Ataki
Abstract Among the heavy metals and other chemicals that contaminate the immediate environment of all gold mining communities, Arsenic and Mercury compounds are some of the most prevalent, exposing residents to their health risks. This menace is the result of the mining activities, particularly, Artisanal and Small-scale gold mining, in these communities. Among the mining areas in Ghana, Artisanal and small-scale gold mining is a recent activity only in the Eastern Region, particularly in the Aduasena, Afosu, Intronang, Hweakwae, New Abirem, Mamano and Hamlets communities. The objective of this research is to investigate the levels of Arsenic and Mercury in the residents of these seven communities using spectroscopic analysis of their urine samples and to identify which gender and at what age does any resident in a typical Ghanaian mining community stand most endangered by the levels of these contaminants. Samples of first urine void of residents upon waking up in the morning were taken, digested with nitric acid and analysed for the concentrations of Arsenic and Mercury using the Perkin Elmer PinAAcle 900T Graphite Furnace AAS. The spectroscopic analysis of the urine samples showed that more than 20% of the residents had concentrations of Arsenic higher than the (normal) recommended level, with some reaching as high as 221 for Arsenic and 3.90 for mercury. Statistical analysis of the results showed that the levels of both Arsenic and Mercury seem to increase with increasing age, despite some extremely high concentrations for arsenic in the Aduasena youth between 31 and 40 years. This trend indicates that males were seen to be more at risk from these contaminants, with the youth between 11 and 20 years standing most endangered.
在污染金矿社区直接环境的重金属和其他化学物质中,砷和汞化合物是最普遍的,使居民面临健康风险。这种威胁是这些社区采矿活动,特别是手工和小规模金矿开采的结果。在加纳的矿区中,手工和小规模金矿开采是最近的活动,仅在东部地区,特别是在Aduasena、Afosu、Intronang、Hweakwae、New Abirem、Mamano和Hamlets社区。本研究的目的是通过对这七个社区居民的尿液样本进行光谱分析,调查他们体内的砷和汞水平,并确定典型加纳采矿社区居民的性别和年龄最容易受到这些污染物水平的危害。采集居民早晨起床后的第一次尿液样本,用硝酸消化,并使用Perkin Elmer PinAAcle 900T石墨炉原子吸收光谱法分析砷和汞的浓度。尿液样本的光谱分析显示,超过20%的居民砷浓度高于(正常)推荐水平,其中砷浓度高达221,汞浓度高达3.90。对结果的统计分析表明,砷和汞的含量似乎随着年龄的增长而增加,尽管在31至40岁的Aduasena青年中砷的浓度极高。这一趋势表明,男性受到这些污染物的威胁更大,其中11至20岁的年轻人最受威胁。
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引用次数: 4
Erratum 勘误表
Pub Date : 2018-01-01 DOI: 10.1080/23312009.2018.1457128
V. E. Tarabanko
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引用次数: 3
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Cogent Chemistry
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