兰索拉唑中有机溶剂残留量的测定

文章建立了采用直接进样毛细管气相色谱法测定兰索拉唑中甲醇、乙醇、乙酸乙酯残留量的方法.色谱柱为HP-FFAP石英毛细管柱,采用程序升温,载气为氮气,检测器为FID,以二氧六环为溶剂.在上述色谱条件下,甲醇的线性范围为6-54mg/L,乙醇和乙酸乙酯的线性范围为10-90mg/L;平均加样回收率分别为99.36、101.26%和101.57%.本方法简便、专属性强、准确度高,可用于测定原料药中甲醇、乙醇、乙酸乙酯的残留量.     

基体改进-石墨炉原子吸收光谱法测定中药丹参中的铜和锌

以 NH4NO3 和 Se Triton X- 10 0作为铜和锌的基体改进剂 ,石墨炉原子吸收法测定丹参中铜和锌的含量。优化了实验条件 ,灰化温度分别提高到 12 0 0℃和 90 0℃ ,提高了方法的灵敏度。研究了不同测定波长对实验的影响 ,消除了基体干扰 ,提高了方法的重现性。用校准曲线法和标准加入法对试样分析结果一致 ,铜和锌的方法检出限分别为 0 .6 ng/ m L和 0 .9μg/ m L,RSD分别为 1.8%和 2 .3% ,回收率分别为 96 %和 10 1%。     

胶束电泳法测定五味子中的3种有效成分

建立了基于一种快速、高效分离与测定五味子中五味子甲素、五味子乙素和五味子酯甲含量的胶束毛细管电泳-紫外检测分析新方法。以毛细管(70cm×50μm i.d×375μm o.d)为分离通道,在最佳电泳介质(30mmol/L SDS,pH=7.2,20mmol/L磷酸盐缓冲溶液)中,当分离电压为21kV时,3种待测物质在11min内达到基线分离。在254nm波长处,五味子甲素、五味子乙素和五味子酯甲的线性响应范围分别为5.0—150.0μg/mL、1.0—100.0μg/mL和1.5—150.0μg/mL;检出限分别为1.0、0.22μg/mL和0.4μg/mL。该方法具有良好的重现性,以100.0μg/mL的五味子甲素、五味子乙素和五味子酯甲测定其保留时间和峰高相对标准偏差(RSD)(n=7)均小于2.98%。本方法用于中药五味子中五味子甲素、五味子乙素和五味子酯甲的含量测定,结果令人满意。     

MPT-AES同时测定航空润滑油中的铝、镁和铜

微波等离子体炬原子发射光谱法 (MPT- AES)测定未使用过的航空润滑油中铝、镁和铜含量。研究了微波功率、载气流量、工作气流量、氧屏蔽气流量、酸效应、共存离子等对元素发射强度的影响 ,优化了系统参数。铝、镁和铜的检出限分别为 15 .1ng/ m L、0 .2 8ng/ m L、2 .1ng/ m L,线性范围分别为 0 .0 5—80μg/ m L、0 .0 0 1— 5 0μg/ m L、0 .0 1— 12μg/ m L ,相对标准偏差均小于 3.7% ,回收率在 95 .6 %— 10 5 .3%之间。方法准确、快速、操作简便、维持费用低。     

ICP-MS测定土壤样品中的有效锰、铜和锌

以DTPA提取土壤中的有效锰、铜、锌,不经分离富集,电感耦合等离子体质谱直接测定土壤样品中的有效锰、铜和锌,方法检出限分别可达0.042μg/L、0.039μg/L、0.028μg/L.通过对国家土壤有效态一级标准物质测试,测定结果基本一致;GBW 07412标准物质11次测定锰、铜和锌的相对标准偏差(RSD)分别为3.49%、3.72%、5.65%.     

Plot-U毛细管柱气相色谱测定工作场所空气中的甲醇

建立了用Plot-U毛细管柱气相色谱测定工作场所空气中甲醇的方法。硅胶管吸附空气中甲醇,水解吸后用Plot-U毛细管柱气相色谱(FID)测定。结果表明,甲醇浓度在0—200μg/mL范围内线性关系良好,线性方程为:y=1.2x-1.2(r=0.9998);检出限为1.4μg/mL,若采集1.5L空气样品,则最低检出浓度为0.9mg/m3;平均加标回收率在90.0%—91.0%之间;相对标准偏差在0.84%—2.60%之间。本方法适用于工作场所空气中甲醇浓度的测定。     

快速声表面波气相色谱技术检测水中苯系物*

建立了便携式声表面波气相色谱快速检测水中苯系物的方法。实验条件:检测器温度25℃,DB-5毛细管色谱柱:初始温度40℃,10℃/s程序升温至180℃。结果表明,氯苯、间二甲苯、苯乙烯、异丙苯保留时间分别为1.72 s、1.86 s、2.00 s、2.22 s,检出限分别为1.34μg/L、0.55μg/L、0.50μg/L、0.39μg/L,测得相对标准偏差值为4.08%~5.98%,回收率为82.7%~103.8%,且线性良好,线性相关系数为0.9946~0.9993。因此,该方法适用于水中苯系物的快速应急监测。     

微波消解-火焰原子吸收光谱法测定下火药材中的微量元素

微波消解样品,火焰原子吸收光谱法测定下火药材中5种微量元素的含量。菊花中钙、镁、铁、锌、锰的含量分别为15.80,31.42,7.68,0.935,0.105g/kg;桑叶中钙、镁、铁、锌、锰的含量分别为195.6,33.69,7.02,0.839,2.21g/kg;夏枯草中钙、镁、铁、锌、锰的含量分别为110.9,38.69,14.75,1.24,0.112g/kg。该方法加标回收率在90.1%—106.3%之间,方法简单、灵敏、准确,可为下火药材的基础研究提供依据。     

荧光偏振免疫分析测定磺胺甲基嘧啶研究

磺胺甲基嘧啶(sulfamerazine,SMR)的芳伯胺基与荧光素异硫氰酸钠异构体Ⅰ(fluorescein isothiocyanate, FITC)的异硫氰基在常温下可以发生偶联反应,经薄层色谱分离之后,可以得到SMR的FITC荧光标记物(Tracer)SMR-FITC。应用荧光偏振免疫分析(fluorescence polarization immunoassay, FPIA),以SMR单克隆抗体为竞争免疫试剂,优化了检测条件,建立了SMR的FPIA检测方法。在选定的条件下,SMR的半数抑制量(IC₅₀)为23.4 ng·mL-1,最低检测限量为2.3 ng·mL-1,检测范围为5.4到218.8 ng·mL-1,可以达到食品中SMR的最高残留限量要求。同时对16种磺胺类药物的交叉反应做了初步研究,结果显示对SMR、磺胺二甲基嘧啶(sulfamethazine, SMZ)、磺胺嘧啶(sulfadiazine, SDZ)交叉反应率分别为100%,25%和8.6%,对其他磺胺类药物的交叉反应率均低于5%。     

FAAS法测定硫酸中的铜、铁和锌

采用火焰原子吸收光谱法测定硫酸中铜、铁和锌,确定了最佳仪器工作条件和样品处理方法.在选择好的实验条件下,测定铜的特征浓度为0.005μg/mL/1%;铁的特征浓度为0.014μg/mL/1%吸收;锌的特征浓度为0.002μg/mL/1%吸收.回收率分别为铜97.7%-98.2%,铁98.2%-99.4%,锌96.8%-98.7%.     

气相色谱法测定二咖啡酰奎尼酸原料药中的有机溶剂残留量

以1,2-二氯乙烷作为内标,气相色谱法定量检测二咖啡酰奎尼酸原料药中7种有机溶剂残留量。色谱柱：DB-624,30m×0.32mm×1.8μm,载气为H2,检测器为FID,采用程序升温的方法。7种残留溶剂的线性关系良好（r〉0.9914）,回收率为92.5%—98.5%,最小检出限量均为0.01%。本方法简便、灵敏、准确,可用于二咖啡酰奎尼酸原料药残留溶剂的质量控制。     

TAME合成原料及产品的气相色谱分析

采用SE- 30毛细柱、FID、程序升温气相色谱法分析了TAME合成原料及产品的C5组成 ,解析出 C5的8个组分 ;采用 GDX1 0 4填充柱、TCD对含醚产品进行了分析 ,解析出水、甲醇及 TAME。为试验研究和工业生产提供了一种快速准确的方法。     

有机溶剂中水的分光光度法测定

在有机溶剂中有水存在时 ,氯醌酸发生离解 ,其最大吸收波长发生红移 ,且吸收强度显著增加。详细地研究了氯醌酸变色机理及其用于测定水的最佳条件 ,建立了一种新的测定有机溶剂中水含量的分光光度分析方法。测定了白酒、食用酒精与试剂无水酒精中的水含量 ,得到满意测定结果。测定线性范围为φ(H2 O) 0 0 2 %～ 10 % ,方法简单、灵敏度高、重现性好。对甲醇、异丙醇、丁酮、丙酮、乙腈、四氢呋喃中水的测定进行了实验 ,得到了相应的吸光度与浓度校准曲线     

Study of various parameters influencing the fixation of metallic ions Cu2+, Zn2+, and Ni2+ at the catalytic Amberlyst-15 resin in the presence of alcohols

The ionic exchange behavior of Zn²⁺, Ni²⁺, and Cu²⁺ metallic ions on Amberlyst-15 commercial resin was studied as a function of resin solution contact time, initial concentration of metallic ions, nature of the solvent, and the amount of resin. The metallic ions were studied in ternary mixtures using both column and batch experiments. In addition, water, methanol, ethanol, and propan-2-ol were used as solvents for dissolving metallic ions. It was found that the resin behavior depends on the solvent nature and the metallic ion concentration. The analysis of solutions by atomic absorption spectrometry revealed that the affinity of the resin for the studied metallic ions followed the sequence Cu²⁺ > Ni²⁺ > Zn²⁺ in the case of an aqueous medium. Furthermore, uptake increased with increasing amount of resin. A better uptake was observed in the case of the 75:25 % water/methanol compositions when the column technique was used. For the batch technique, we noted a better uptake using 100 % water. The uptake rate decreased with an increase in the number of carbons for the 50 % water–50 % alcohol solvents. The acid–base properties of Amberlyst-15 commercial resin were studied by 2-propanol decomposition test. Propene and acetone are the main expected products and it is believed that they are formed through dehydration or dehydrogenation reaction on acid and base sites, respectively.     

气相色谱法测定番茄酱中菊酯类农药的残留量

首次建立了番茄酱中氯氰菊酯、氰戊菊酯和溴氰菊酯的提取、净化及气相色谱测定方法,农药残留运用混合溶剂提取,填有Ｆｌｏｒｉｓｉｌ的层析柱净化,电子捕获－气相色谱法检测。本方法的回收率为８２．６％－８８．１％,检出限为０．０５ｍｇ／ｋｇ。     

Influence of the Solvent on the Formation of CNR/BNR Polymer Blends

Structural dynamic analysis combining IR spectroscopy, DSC, and EPR spectroscopy is applied to studying films based on chlorinated natural rubber (CNR), butadiene nitrile rubber (BNR), and blends thereof. The influence of various solvents, such as methyl ethyl ketone (MEK), ethyl acetate (EA), methyl acetate (MA), and acetone (A), on the structure and molecular dynamics (τ) of CNR/BNR polymer films is examined. The strongest changes in the molecular mobility (τ) and the glass transition temperature (T_gt) relative to those of the starting materials are observed for the 50: 50% CNR/BNR blends prepared using all the solvents (except for acetone, the maximum values of τ for which is observed at a ratio of CNR: BNR = 80: 20%), which can be explained by the inversion of phases in the blends. Annealing at 140°С causes an increase in the correlation time of the probe, and, consequently, a decrease in the molecular mobility, which is due to the intermolecular crosslinking of the components.     

Effect of pure and mixed solvents on the solubility, crystal growth and morphology of ethyl p-dimethylamino benzoate (EDMAB): An organic nonlinear optical material

The effects of pure and mixed solvents of ethanol and acetone on solubility, nucleation and growth of ethyl p-dimethylamino benzoate (EDMAB) were investigated. It was found that solubility of EDMAB increased as the volume ratio of acetone increased in the mixed solvent. Growth experiments were performed at 32 °C using pure and mixed solvents with different volume ratios of ethanol and acetone. Bulk single crystals of EDMAB were grown-in the experiment conducted using mixed solvent of 25% acetone and 75% of ethanol, whereas thin platelet crystal of EDMAB was obtained in the experiment conducted using pure ethanol. The acetone rich system resulted in uncontrolled nucleation with large number of tiny crystals, possibly due to high vapor pressure of acetone. The grown crystals were subjected to various analytical studies such as powder X-ray diffraction, Vickers microhardness, dielectric studies as a function of frequency and optical transmission and the powder Kurtz method.     

Fluorescence and Time-Resolved Delayed Luminescence of Porphyrins in Organic Solvents and Polymer Matrices

Porphyrin dyes fulfill an essential function in photosynthesis and are important in photodynamic therapy and in a range of electronic devices. Their spectroscopic characteristics may play a crucial role in these processes. The spectral properties of two porphyrin dyes: tetraphenylporphyrin and tetraphenysulfporphyrin in organic solvents (acetone, chloroform, methyl alcohol, and dimethyl-sulfoxide) and in polyvinyl alcohol and poly(methylmethacrylate) films have been investigated. Absorption, fluorescence, and microsecond time-resolved delayed luminescence spectra have been measured at room temperature. The existence of different aggregated dye forms in the ground and excited states has been demonstrated. The manifold of dye species depends on the solvent/polymer. In the case of the polymers, it also depends on the solvent used to coat the polymer film. Delayed luminescence spectra and decay times of the two porphyrins in the different solutions and in polymeric matrices suggest that different mechanisms of deexcitation of the singlet excited states may be responsible for their generation in these and other porphyrin dyes.