X-射线荧光光谱铝环-双层压片法测定少量土壤中的化学元素

本文提出用铝环一双层压片法制备样片,经验系数法校正元素间效应,对少量土壤样品中的化学元素进行定量测定。取样量500mg,制样与测量精度小于5％,用本法对标样的分析表明,分析值与推荐值基本一致,本法具有简单、快速、成本低的特点,适用于少量样品的分析。     

透明胶纸制样法X—射线荧光光谱测定蒙脱石中的化学元素

本文提出以透明胶纸作为少量粉末样品的支持物来制备样片,采用透空照射法,在日本理学3080E3型X-射线荧光光谱仪上实现了蒙脱石中化学元素的定量测定。本法样品实际用量约10mg,制样与测量精度较好,标样及样品的分析结果与推荐值及AAS法分析结果基本一致,方法具有简单、快速、准确和成本低的特点,适用于少量样品和单矿物的分析。     

大洋底多金属结核样品中主、次、微量元素的X射线荧光光谱测定

制定了一个用X射线荧光光谱法测定大洋底多金属结核样品中主、次、微量元素的分析方法。样品用石墨坩埚、混合熔剂低倍稀释熔融,用人工标样作为校准标准。计算了COLA方程的理论α系数,用于校正28个分析元素的吸收-增强效应。本法测定结果与化学法结果相吻合。     

矿石中铀的精密电位滴定

本文提出的精密电位滴定法,采用HF-HNO_3-HClO_4溶矿,不过滤、不分离,缩小了滴定液的体积;同时还重视了电极对滴定精度的影响,提出了有效的处理方法;在确定终点所消耗的NH_4VO_3体积时,采用二次电位差分法进行精确计算,提高了方法的精密度。本法对铀矿石标准样品和铀矿石样品的分析,其准确度和精密度均小于±1.5％。操作步骤 1.样品处理:准确称取矿样1.000～2.000g于100ml聚四氟乙烯烧杯中,用少量水湿润,加5～     

原子吸收分光光度法测定生物样品中的游离脂肪酸

本文研究了用原子吸收分光光度法间接测定生物样品中游离脂肪酸(FFA)的方法,用氯仿-正己烷-甲醇混合液萃取样品中FFA,用铜溶液与FFA形成“铜皂”,进入有机相,未反应的Cu~(2+)进入水相,用原子吸收法测定有机相中铜,间接求得游离脂肪酸含量。本法线性范围为10～100nmol,对血浆测定结果的相对标准偏差为<6.59％,回收率为96％～102％。本法的测定结果与比色法的结果基本一致。     

火焰原子吸收光谱法测定家禽卵中痕量铜、铅、锌、镉、锰、铁

本文就家禽卵中痕量重金属的火焰原子吸收法测定作了一些探讨,找出硝酸与硫酸按3∶1混合在150℃左右可将高蛋白,高脂肪样品进行消解的条件,分析程序安全、快速、准确,适宜日常大量高蛋白,高脂肪环境样品分析。有机样品消解文献多用干法,湿法两种。干法费时过长,对工作区周围空气污染严重;温法使用混合溶剂:硝酸-硫酸-高氯酸,硝酸-高氯酸,硝酸-硫酸,硝酸-过氧化氢,或用玻璃棉将脂肪过滤等复杂手续。而高蛋白、高脂肪样品用高氯酸消解时最易引起爆炸,Haig Agemian等提出用硝酸-硫酸-过氧化氢法消解高脂肪、高蛋白样品,虽避免使用高氯酸,然而用过氧化氢澄清炭黑时,过氧化氢用量太多。本法用硝酸-硫酸消解家禽卵,直接     

偶氮氯膦Ⅲ螯合形成树脂分离富集ICP发射光谱测定地质样品中15个稀土元素

本文重点报道用CPA-Ⅰ试剂溶液与D_(290)大孔强碱性阴离子树脂经简单搅拌而制得的CPA-Ⅰ整合形成树脂,分离岩石中基体元素,富集稀土元素,然后用ICP-AES法测定15个稀土分量。实验表明,在一定量乳酸、EDTA-Zn及抗坏血酸存在下,于pH_1-1.5,15个稀土元素的回收率均在94-106％之间,柱上分离时间约两小时,相对标准偏差<5％。分析标准沉积物及岩石样品本法所得结果与推荐值满意地一致。     

X荧光滤纸片薄样法测定铅锌矿选矿流程样中Pb,Zn,Cu,Fe

本法将Ｘ荧光滤纸片薄样法用于具有复杂组分的铅锌矿选矿样品中Ｐｂ，Ｚｎ，Ｃｕ，Ｆｅ的分析，样品经化学溶样后滴于定量滤纸片上，标准样品可直接用纯试剂人工配制，用同样制成滤纸片薄样标准系列，因薄样测定可不作基体效应校正，标样使用数量少，又无需化学法标定。故方法实验周期短，样品测定手续简便快速，元素分析含量适应范围宽，可适用于组分复杂，元素含量变化范围大的试样分析，样品分析结果与化学法相符，方法准确度与精     

分光光度法快速测定毒鼠强的研究

本文将毒鼠强在酸性条件下分解,分解产生的甲醛用水蒸汽蒸馏使之与干扰物质分离,再根据Hantzsch反应原理,用乙酰丙酮-乙酸铵溶液作显色剂分光光度法测定甲醛,从而间接测定毒鼠强的含量。本法的线性范围为5~40 mg/kg。本法干扰少,操作简便、快速,可用于中毒样品的测定。     

装饰用焊接不锈钢管镍含量的快速测定

采用空气-乙炔火焰原子吸收光谱法快速测定装饰用焊接不锈钢管的镍含量,测定波长为232.0nm。试验数据表明,本法对样品测定结果的相对标准偏差小于4％,在国家标准GB／T223、25-1994方法规定的重复性范围内,对标准样品测定结果与国标法测定结果的偏差满足规定要求。检测耗时约是GB／T223.25-1994方法的1／5。本方法是一种实用、高效、准确地测定装饰用焊接不锈钢管中镍含量的方法。     

Continuous concentration of bacteria in a microfluidic flow cell using electrokinetic techniques

A novel method for the concentration of bacterial solutions is presented that implements electrokinetic techniques, zone electrophoresis (ZE) and isoelectric focusing (IEF), in a microfluidic device. The method requires low power (< 3e-5 W) and can be performed continuously on a flowing stream. The device consists of two palladium electrodes held in a flow cell constructed from layers of polymeric film held together by a pressure-sensitive adhesive. Both ZE and IEF are performed with carrier-free solutions in devices in which the electrodes are in intimate contact with the sample fluid. IEF experiments were performed using natural pH gradients; no carrier ampholyte solution was required. Experiments performed in buffer alone resulted in significant electroosmotic flow. Pretreatment of the sample chamber with bleach followed by a concentrated solution of cationic detergent effectively suppressed electroosmotic flow.     

Optimization of a flow injection analysis system for tartaric acid determination in wines

The objective of this work is the development and optimization of a method for tartaric acid analysis in wines that does not require any sample pre-treatment and with adequate accuracy. A flow injection analysis manifold with three channels, using a dialysis unit to eliminate sample matrix interferences and to accomplish on-line dilution, is proposed for the spectrophotometrical determination of tartaric acid in wines making use of its reaction with vanadate. The proposed method is fast, accurate, simple, economic and does not require any sample pre-treatment. Preliminary studies using factorial designs were performed to determine which operational parameters should be included in the optimization stage. The optimization was performed using a modified simplex algorithm with a response function that included sensitivity, deviation from linearity at low concentrations and residence time, used as an inverse measure of sampling rate. The most relevant analytical parameters of the method are presented, including a comparison between the results provided by the proposed method and by an alternative procedure in the analysis of a set of wine samples from Portugal, with tartaric acid values in the range 0.5–4 g l⁻¹.     

Determination of sodium dodecylbenzene sulfonate in ternary mixtures by curie-point pyrolysis gas chromatography coupled to multivariate analysis

Summary Multivariate analysis was used to develop a viable method for determination of sodium dodecylbenzene sulfonate (DBS) by Curie-point pyrolysis gas chromatography. The pyrograms obtained were normalized against a maximum peak area and peak height. Normalized values were used for Quantification IV, which is one of the multivariate analysis methods, to select useful values initially. Then cluster analysis was carried out using both the selected values and their deviations. This method corresponds to qualitative analysis and indicates which data-base is similar to the sample. On the basis of this data-base, calibration data-bases are chosen. Principal component analysis (PCA) was performed using the calibration data-base and a set of sample data simultaneously. The principal component scores and contribution coefficients obtained were used to construct a calibration curve from which the DBS content of the sample was calculated. The results are in fair agreement with theoretical values.     

Single‐step CE for miniaturized and easy‐to‐use system

We developed a novel single‐step capillary electrophoresis (SSCE) scheme for miniaturized and easy to use system by using a microchannel chip, which was made from the hydrophilic material polymethyl methacrylate (PMMA), equipped with a capillary stop valve. Taking the surface tension property of liquids into consideration, the capillary effect was used to introduce liquids and control capillary stop valves in a partial barrier structure in the wall of the microchannel. Through the combined action of stop valves and air vents, both sample plug formation for electrophoresis and sample injection into a separation channel were successfully performed in a single step. To optimize SSCE, different stop valve structures were evaluated using actual microchannel chips and the finite element method with the level set method. A partial barrier structure at the bottom of the channel functioned efficiently as a stop valve. The stability of stop valve was confirmed by a shock test, which was performed by dropping the microchannel chip to a floor. Sample plug deformation could be reduced by minimizing the size of the side partial barrier. By dissolving hydroxyl ethyl cellulose and using it as the sample solution, the EOF and adsorption of the sample into the PMMA microchannel were successfully reduced. Using this method, a 100‐bp DNA ladder was concentrated; good separation was observed within 1 min. At a separation length of 5 mm, the signal was approximately 20‐fold higher than a signal of original sample solution by field‐amplified sample stacking effect. All operations, including liquid introduction and sample separation, can be completed within 2 min by using the SSCE scheme.     

Characterization of trace elements in high viscosity materials by total reflection X-ray spectrometry

This paper proposes the use of radiation scattered by the sample instead of the internal standard method for quantifying impurities in high viscosity materials using X-ray fluorescence with total reflection geometry. The method has been performed for checking trace elements in gels of polymers. Advantages include no sample preparation and a minimum amount of sample (10 μl). The method is also insensitive to instrumental variations, sample amount and particle size of the sample. The ratio of coherent to incoherent scattering intensities of X-ray was also investigated to estimate the content of C plus O in these polymers.     

Determination of sodium azide in beverages by ion chromatography

A convenient method for determination of sodium azide in beverages using ion chromatography is described. This method combines the specificity for azide with a simple sample preparation using a bubble and trap apparatus that removes any interferences. Sodium azide in a sample was acidified, and the azide was converted to the volatile hydrazoic acid, which was trapped in 2.5 mM sodium hydroxide solution. Determination was performed by isocratic ion chromatography using suppressed conductivity detection. Calibration curves were linear for 0.5 to 20 microg/mL sodium azide and the detection limit was 0.05 microg/mL. Recoveries of sodium azide from spiked samples (10.0 microg/g) were more than 82.6%. The method was then used to analyze various beverages.     

Validation of an analytical method using HPLC–MS/MS to quantify osimertinib in human plasma and supplementary stability results

A new method for quantification of osimertinib (OSIM) in human plasma using a high-performance liquid chromatography–tandem mass spectrometry method was developed and validated. Methanol was used for protein precipitation and pazopanib as internal standard. Separation was performed on a HyPURITY®C₁₈ analytical column (50 × 2.1 mm; 3 μm) using a gradient elution of ammonium acetate in water and ammonium acetate in methanol, both acidified with formic acid 0.1%. Detection and quantification of OSIM and pazopanib was performed using a triple quadruple mass spectrometer after electrospray ionization. This method led to robust results, as the selectivity, carryover, precision and accuracy all met pre-specified requirements. OSIM was stable in human serum when stored at −80°C. Reduced stability was found when stored at 2–4°C or room temperature. Degradation of OSIM slowed down in EDTA–plasma and acidified human serum. The limited stability of OSIM at room temperature should be considered for transport and sample preparation. Plasma samples should be frozen as soon as possible and sample preparation should be performed on dry-ice. In the future, EDTA–plasma and sample acidification may be used to improve OSIM stability at room temperature. However, more research and validation of such an approach are required.     

反相离子对液相色谱法测定欧洲鳗鲡体中丙硫咪唑及其代谢物的残留量

建立了鳗鲡体中丙硫咪唑及其代谢物残留量测定方法。样品用乙腈提取,经正己烷净化后,液相色谱一荧光法测定,标准加入法定量。流动相为：甲醇、乙腈和乙酸铵,梯度洗脱。检测波长为：激发波长290nm,发射波长320nm,丙硫咪唑、2氨基丙硫咪唑砜、丙硫咪唑亚砜、丙硫咪唑砜检出限依次为：25、5、10、1μg／kg。回收率大于95％,相对标准偏差小于8％。     

Optimal flip angle for robust practical quantitative NMR measurement using a fixed pulse length

NMR quantification has been traditionally performed by using internal standards. Although methods using external reference in NMR quantification have been developed, the major obstacles in using external referencing method are the measurement deviations associated with changing sample conditions and the requirement of pulse width calibration for every sample in order to compensate these errors. The calibration process is time consuming and in some cases impossible. We developed a quantitative NMR method fixed pulse length (FIXPUL) for all measurements without sample-by-sample calibration. The method is based on the use of an optimal flip angle calibrated for an external standard so that the quantitative errors associated with the pulse width variations are minimized. FIXPUL can be implemented on most basic NMR spectrometers and is robust and easily automated. The method is applicable to a wide range of solution NMR samples in chemistry, biology, and drug research and discovery.     

A novel injection method for high-speed proteome analysis by capillary electrophoresis

We have developed a new sample injection method for capillary electrophoresis (CE) that reduces the required migration time. We demonstrated a pressurization technique that was performed with buffer in the outlet after the electrokinetic sample injection with no buffer in the outlet. To reduce the migration time, the sample injection had to be performed with no buffer in the outlet; water should be pressurized while the buffer is in the outlet. Though the resolution was slightly decreased using this method, the addition of a separation carrier (curdlan) to the run buffer restored the resolution without delaying the migration time. The use of our new sample injection method combined with our high-quality separation carrier will enable us to improve the efficiency of the high-throughput screening (HTS) system for proteome analysis.