高效液相色谱法测定氧氟沙星含量的方法改进

对高效液相色谱法（HPLC）测定氧氟沙星原料药含量的方法改进。在氧氟沙星原料药含量测定结果与印度药典方法无显著差异条件下,大大缩短了分析时间。本方法快速、准确,更适用于常规检验工作和厂方大批量生产时的质量控制。     

高效液相色谱法测定化妆品中的保泰松

建立了化妆品中保泰松的高效液相色谱分析法.采用甲醇超声提取样品,氨基固相小柱净化富集,以C18色谱柱(4.6 mm×250 mm,5μm)分离,流动相为20 mmol/L乙酸铵水溶液、甲醇和乙腈,流速1.0 mL/min,检测波长270 nm,柱温25℃,进样量10 μL.该方法的检出限为2.0 mg/kg,线性范围0.2～100.0μg/mL,加标回收率86.1％ ～90.5％,相对标准偏差为5.79％～9.21％.     

粉葛HPLC指纹图谱研究中有效成分提取条件的优化

为了优化粉葛HPLC指纹图谱研究中有效成分的提取条件,采用梯度洗脱(0～50 min A相由20%升为55%),流动相甲醇-乙腈(70∶30)(A)和水(B),柱温35℃,流速0.6 mL/min,检测波长268 nm的色谱条件监测,比较方法、溶剂种类及浓度、时间、溶剂用量比例等提取条件。结果表明,以30%甲醇溶液作为溶剂,超声30 min(40℃,70 Hz),125倍溶剂用量比例时,提取稳定性好、提取效率高,可作为粉葛HPLC指纹图谱分析的较优条件。     

乙撑硫脲在人参茎叶中的残留动态

[方法]通过田间试验和液相色谱分析技术研究了75％代森锰锌代谢物乙撑硫脲在茎和叶中残留动态和最终残留量.[结果]吉林抚松田间试验结果表明:施药剂量为推荐剂量的2倍(6250 g a.i./hm2)时,乙撑硫脲在茎和叶中原始沉积量分别为0.782、8.23 mg/kg;半衰期分别为4.9、19.5 d.施药1次,测得茎中乙撑硫脲残留量14d后低于欧洲规定的MRL值(0.05 mg/kg),而叶中乙撑硫脲残留量均高于欧洲规定的MRL值(0.05 mg/kg).[结论]综合多方面因素,按照推荐剂量3 125 g a.i./hm2处理,建议我国在茎上乙撑硫脲的MRL值可暂定为0.05 mg/kg,茎安全间隔期为14 d,而叶上的残留量较高,建议MRL值可暂定为0.50 mg/kg,叶安全间隔期无法确定,施药次数为1次.     

浅谈液相色谱仪的管理与维护

介绍了高效液相色谱仪的结构组成和发展,阐述了流路泵系统、色谱柱和几种常用检测器的管理与维护,为液相色谱分析工作,提供一些值得借鉴的仪器管理与维护经验。     

HPLC在中药分析中的应用

中药化学成分复杂,其成分分析一直存在着分离难度大、分析时间长等问题,高效液相色谱法（HPLC）是中药质量分析最重要的手段之一。综述了HPLC在中药化学成分分析中的应用。     

高效液相色谱测定三苯基乙酸锡在水稻中的残留

[目的]建立三苯基乙酸锡在水稻植株和土壤中残留量的高效液相色谱检测方法。[方法]样品用乙腈提取后,二氯甲烷萃取,经酸性氧化铝柱净化,以乙腈-0.5%磷酸水(体积比30∶70)为流动相,用紫外检测器测定。[结果]水稻植株和土壤样品中三苯基乙酸锡的添加平均回收率分别为86.4%～102.9%、88.8%～105.2%,相对标准偏差分别为5.1%～10.2%、2.4%～8.3%,最小检出量为1.0×10-10 g,最低检测质量分数为2.0×10-3 mg/kg。[结论]方法操作简便,符合农药残留分析的要求,为其他作物中三苯基乙酸锡残留量的测定提供参考。     

Molecularly imprinted polymers: present and future prospective

Molecular Imprinting Technology (MIT) is a technique to design artificial receptors with a predetermined selectivity and specificity for a given analyte, which can be used as ideal materials in various application fields. Molecularly Imprinted Polymers (MIPs), the polymeric matrices obtained using the imprinting technology, are robust molecular recognition elements able to mimic natural recognition entities, such as antibodies and biological receptors, useful to separate and analyze complicated samples such as biological fluids and environmental samples. The scope of this review is to provide a general overview on MIPs field discussing first general aspects in MIP preparation and then dealing with various application aspects. This review aims to outline the molecularly imprinted process and present a summary of principal application fields of molecularly imprinted polymers, focusing on chemical sensing, separation science, drug delivery and catalysis. Some significant aspects about preparation and application of the molecular imprinting polymers with examples taken from the recent literature will be discussed. Theoretical and experimental parameters for MIPs design in terms of the interaction between template and polymer functionalities will be considered and synthesis methods for the improvement of MIP recognition properties will also be presented.     

Rapid and Green Analytical Method for the Determination of Quinoline Alkaloids from Cinchona succirubra Based on Microwave-Integrated Extraction and Leaching (MIEL) Prior to High Performance Liquid Chromatography

Quinas contains several compounds, such as quinoline alkaloids, principally quinine, quinidine, cinchonine and cichonidine. Identified from barks of Cinchona, quinine is still commonly used to treat human malaria. Microwave-Integrated Extraction and Leaching (MIEL) is proposed for the extraction of quinoline alkaloids from bark of Cinchona succirubra. The process is performed in four steps, which ensures complete, rapid and accurate extraction of the samples. Optimal conditions for extraction were obtained using a response surface methodology reached from a central composite design. The MIEL extraction has been compared with a conventional technique soxhlet extraction. The extracts of quinoline alkaloids from C. succirubra obtained by these two different methods were compared by HPLC. The extracts obtained by MIEL in 32 min were quantitatively (yield) and qualitatively (quinine, quinidine, cinchonine, cinchonidine) similar to those obtained by conventional Soxhlet extraction in 3 hours. MIEL is a green technology that serves as a good alternative for the extraction of Cinchona alkaloids.     

Efficient electrochemical decomposition of perfluorocarboxylic acids by the use of a boron-doped diamond electrode

The electrochemical decomposition of environmentally persistent perfluorooctanoic acid (PFOA) was achieved by the use of a boron-doped diamond (BDD) electrode. The PFOA decomposition follows pseudo-first-order kinetics, with an observed rate constant (k₁) of 2.4 × 10^− 2 dm³ h^− 1. Under the present reaction conditions, k₁ increased with increasing current density and saturated at values over 0.60 mA cm^− 2. Therefore, the rate-limiting step for the electrochemical decomposition of PFOA was the direct electrochemical oxidation at lower current densities. In the proposed decomposition pathway, direct electrochemical oxidation cleaves the C-C bond between the C₇F₁₅ and COOH in PFOA and generates a C₇F₁₅ radical and CO₂. The C₇F₁₅ radical forms the thermally unstable alcohol C₇F₁₅OH, which undergoes F⁻ elimination to form C₆F₁₃COF. This acid fluoride undergoes hydrolysis to yield another F⁻ and the perfluorocarboxylic acid with one less CF₂ unit, C₆F₁₃COOH. By repeating these processes, finally, PFOA was able to be totally mineralized to CO₂ and F⁻. Moreover, whereas the BDD surface was easily fluorinated by the electrochemical reaction with the PFOA solution, medium pressure ultraviolet (MPUV) lamp irradiation in water was able to easily remove fluorine from the fluorinated BDD surface.