新型高效杀虫剂甲氰菊酯及其制剂的气相色谱分析

甲氰菊酯(Fenpropathrin),商品名为Meotherm,是一种合成的广谱、高效的拟除虫菊酯类杀虫剂。为了配合甲氰菊酯的合成研究及工业开发,我们在国内首次建立了反相高效液相色谱法。本文报告我们建立的适于工业生产检测的气相色谱定量分析方法。     

哌嗪及其共生物的气相色谱分析研究

研究了哌嗪及其共生物的气相色谱分析方法。采用Chromsorb WAW（60～80目）为担体,以氢氧化钾作减尾剂,聚乙二醇（PEG 2万）作固定液,在长 1.5m的玻璃填充柱上哌嗪及其共生物得到良好的分离。除乙二胺外,其他相对误差均小于2％。并且计算了哌嗪及其共生物的得率和原料的转化率。     

烯效唑及其中间体Z、E构型三唑烯酮的气相色谱分析

1引言烯效唑（pentefezol）是新型的高效、广谱、低毒植物生长延缓刑。化学名称为1-对氯苯基-2-（1，2，4-三唑-1-基）－4，4-二甲基-戊烯-3-醇，其结构中3号碳为手性碳，1，2-碳碳双键连接4个不同基团，说明烯效唑既有旋光异构体，又有几何异构体，其中E-型控长活性大大高于I-型，S-型，一般高于R-型。所以合成稀效唑尽可能获得高效的S-E型的异构体，而选获得Z、E-三唑烯酮并实现从型转化优势是关键。测定烯效唑及其中间体三唑烯酮一般用液相色谱法，但无法解决识别Z、E构型的难题。如能用同类方法、同台仪器、甚至同一色谱柱既可测定…     

苯系物的色谱分析方法的研究进展

对近几年来苯系物的色谱分析方法的研究进展进行了综述,着重介绍了气相色谱内标法以及顶空、固相微萃取、液液微萃取等前处理方法,并对苯系物的分析发展方向和控制进行了展望(引用文献49篇)。     

蛇床子挥发油的提取方法及其化学成分的气相色谱分析

中药药材蛇床子为伞形科植物蛇床子的干燥成熟果实,别名蛇米、野胡萝卜子、野茴香。果皮松脆,种子细小,灰棕色,显油性;气香,味辛凉,有麻舌感。蛇床子的挥发油在临床上具有止咳、平喘、祛痰、发汗、解表、祛风、镇痛、解热、利尿、健胃、抗菌、消毒、杀虫等功效;还用于治疗阳萎、宫冷、寒湿带下、湿痹腰疼等,可抗诱变与抗癌、抗变态反应、提高免疫力、延缓衰老、美肤美容等不同的功能;工业还用于制造香料和指示剂等。文献对于蛇床子中挥发油的成分已有报道,但因蛇床子挥发油的成分复杂,且产地不同,因此结果也有明显的差异。采用水蒸气蒸馏法和挥发油提取器提取法来提取蛇床子中的挥发油,得到最佳的提取蛇床子挥发油的方法。对蛇床子挥发油深入研究不仅可以揭示该植物的生长环境和化学成分的关系,还为进一步开发和利用新药资源提供了科学依据。     

钻井液中烃类气体的色谱分析进展

最近几年，人们开始关注泥浆气体地面监测问题，原因是气体探测技术的进步和地面监测成本的下降。     

色谱分析中样品前处理技术的发展动态

作为现代分析领域的重要手段之一,色谱可用于食品、环境、生物等复杂样品的定性与定量分析。而样品前处理是获得理想色谱分析结果的必要前提,它可有效消除基质干扰、浓缩目标分析物、改善分离效能以及延长色谱仪器使用寿命。本文主要依据2020年4-5月Anal Chem新发表和在线录用的有关论文,讨论色谱分析中涉及样品前处理技术方面的最新发展动态。     

样品前处理-色谱分析在线联用技术的研究进展

样品前处理是色谱分析中耗时最多、最容易引起误差的关键环节,因此有关样品前处理技术与色谱分析的在线联用的研究已成为分析化学的前沿课题。本文综述了近年来各种样品前处理技术与色谱分析在线联用的研究进展,包括固相萃取、固相微萃取与液相微萃取、膜辅助萃取、场作用辅助萃取、气相萃取、热解吸以及微芯片分离技术。     

大气颗粒物中有机物色谱分析的样品制备技术

大气颗粒物中有机物成分分析对深入研究大气颗粒物对人类健康、环境、气候、生态的影响,解析气溶胶来源,制定颗粒物控制相关法规,以及风险管理方法具有重要意义。由于颗粒物中的有机组分种类繁多,分析复杂,目前仅10%~20%的有机物得到了定性和定量分析。因此,大气细颗粒中有机物的分析已成为环境分析领域的优先发展方向。色谱是大气颗粒物中有机物分析的主要方法,而样品制备则是影响分析速度和精度的关键步骤。本文对颗粒物中有机组分色谱分析前的样品制备方法进行了综述,介绍了索氏提取、超声辅助提取、微波辅助提取、加压溶剂提取等溶剂提取方法以及热解吸提取方法,并重点介绍了这些方法在大气颗粒物样品处理中的应用,总结了各种方法的优缺点。     

A history of thermochemistry through the tribulations of its devotees

The history and the evolution of thermochemistry are covered in a number of excellent books. In order not to repeat what has already been written, this paper will be concerned with thermochemists as persons through their odd stories and anecdotes, of hot, enduring and even fierce debates, of accidents in the laboratory. This revised version was published online in July 2006 with corrections to the Cover Date.     

Studies in the history and development of thermogravimetry

Several examples of the earliest commercial thermal analysis apparatus, the Talabot-Persoz-Rogeat Desiccator, are exhibited in various French museums and there is documentary evidence that at least twelve were exported to the UK in the late 19th Century. This paper describes the search for extant examples in the UK.     

Preparative scale mass spectrometry: A brief history of the calutron

Calutrons were developed in the laboratory of E. O. Lawrence at the University of California at Berkeley. They were a modification of the cyclotrons he had invented and used in his Nobel Prize‐winning investigations of the atomic nucleus. At the time their construction was undertaken, calutrons represented the only certain means of preparing enriched uranium isotopes for the construction of a fission bomb. The effort was successful enough that every atom of the 42 kg of ²³⁵U used in the first uranium bomb had passed through at least one stage of calutron separation. At peak production, the first stage separators, α tanks, yielded an aggregate 258‐g/day ²³⁵U enriched to about 10 at. % from its natural abundance level of 0.72 at. %. The second stage separators, β tanks, used the 10 at. % material as feedstock and produced a total 204‐g/day ²³⁵U enriched to at least 80 at. %. The latter, weapons grade, material was used in fission bombs. Under typical operating conditions, each α tank operated at a uranium beam intensity at the collectors of approximately 20 mA and each β tank at a beam intensity of approximately 215 mA at the collectors. Bulk separation of isotopes for bomb production ceased in 1945. Since that time calutrons have been used to separate stable isotopes, but on a more limited scale than wartime weapons production. Stable isotope separations since 1960 have taken place using one modified β tank.     

On the history of the development of Sephadex®

Summary The creative and stimulating atmosphere in the laboratories of The Svedberg and Arne Tiselius in the Departments of Physical Chemistry and Biochemistry of Uppsala University during the 1930's, 1940's and 1950's, was a nursery for a remarkable set of both academic and industrial advances. Their pupils were to become distinguished professors at Swedish Universities, as well as abroad, and they were directly involved in the development of two successful Swedish industries, LKB-produkter AB in Stockholm and Pharmacia AB in Uppsala. This review describes the preconditions and the events which led to the development of one of the first commercially available biochemical separation products, the gel filtration medium Sephadex which was introduced by Pharmacia AB in 1959. All the necessary components of a successful transfer of academic research to industrial product development were at hand: a scientific culture of common origin and a longstanding tradition in methodological research; mutual understanding and respect combined with informal links not only between the scientists involved but also between the president of the company and the university authorities. So far, 49 products (excluding those intended for use in health care and diagnostics) have been developed based on the epichlorohydrin cross-linked dextran gel Sephadex. This review is dedicated to my teacher professor Jerker Porath on his retirement as Jacobsonian Professor of Biochemistry at Uppsala University in December 1987.     

Determination of anthraquinones in Rhamnus purshiana using high-performance liquid chromatography coupled to diode array detector and simple ultraviolet spectroscopic analysis

A new method based on Ultraviolet spectrophotometry was developed and compared with that based on high-performance liquid chromatography for the determination and quantification of anthraquinones in the extracts of Rhamnus purshiana bark. A validated quantitative analysis of cascaroside A, cascaroside B, emodin, and aloe-emodin in these herbal products has been previously performed using high-performance liquid chromatography coupled with a diode array detector. In the high-performance liquid chromatography analysis, all the anthraquinones showed satisfactory regression (r² > 0.98) within the test ranges, and the recovery was in the range of 94–117%. The limits of detection and quantification were 0.008–0.010 and 0.029–0.035 μg/mL, respectively. Hierarchical cluster analysis and principal component analysis showed differences in the anthraquinones determined from herbal samples. Subsequently, a simple and low-cost ultraviolet spectrophotometric methodology for the quantitative analysis of the same compounds in the extracts was applied, and all the contents were determined. A paired t-test confirmed that there were no significant differences between the two methods. Our results revealed that the developed method is simple and provides the ability to discriminate and control the quality of anthraquinones in herbal products.     

Analytical method development and validation of anticancer agent, 5-fluorouracil,and its metabolites in biological matrices: An updated review

Abstract

5-fluorouracil (5-FU) refers to a fluorinated pyrimidine analogue that has been widely used as an anticancer agent for colon, head, and neck cancers. Detection of 5-FU and its metabolites; 5-fluorouridine and 5-fluoro-2-deoxyuridine in biological samples allows optimization of pharmacotherapy and encourages fundamental investigations of this medication. The development of accurate and reliable sample preparation, as well as analytical methods, is critical to isolate targeted analytes from complex matrices, apart from increasing detection sensitivity of analytes. With that, this paper presents a review of prior studies pertaining to chromatographic and electrophoretic methods that focused on the analysis of 5-FU and its metabolites in biological matrices such as plasma and urine. This paper concentrates on HPLC, GC and CE systems, which are the most commonly used strategies for analytical separation of 5-FU and its metabolites from samples. Detection of these antineoplastic agents at trace level demands highly sensitive and selective analytical methodologies. Application of these analytical techniques to biological matrices is reviewed with a focus on method development strategies, including types of mobile phases and background electrolytes employed in LC and CE systems.     

色谱数据可视化及天然植物药指纹特征发现方法

提出一类色谱分析数据可视化方法,并用于发现天然植物药的化学指纹特征。选取中药材川芎作为典型研究对象,采用核主成分分析和空间投影变换法对色谱分析数据进行预处理,提取特征信息,再利用二维灰度映像对变换后的数据进行可视化表达,发现其化学指纹特征,从而直接反映出药材质量类别间的化学模式差异。将该方法用于辨识34个不同产地及等级的川芎样品,结果令人满意,证明其具有视觉模式分辨优点,是表达隐含特征指纹和辨识复杂化学物质体系的有力工具。     

基于有限脉冲响应滤波器的实时小波算法及其在色谱信号解析中的应用

对色谱信号进行正确、实时地解析是利用色谱仪器系统进行过程检测的关键技术。小波分析方法能对色谱信号进行有效解析,但实时性一直是制约该方法在色谱信号处理中广泛应用的一个瓶颈。多分辨率分析与重构算法(MALLAT)是小波分析的一种快速算法,但是该算法的实时性仍然需要进一步提高。针对这一问题,以MALLAT算法原理为基础,利用在分解重组过程中两组滤波器系数之间的关系提出了一种基于有限脉冲响应滤波器的实时小波分析算法。仿真结果表明,与经典的MALLAT小波快速算法相比,该算法在保持信号有效分解与重构的基础上,运行耗时明显缩短,实时性得到较大提高。     

Ultra‐performance liquid chromatography tandem mass spectrometry for the rapid,simultaneous analysis of ziprasidone and its impurities

The separation and characterization of the unknown degradation product of second‐generation antipsychotic drug ziprasidone are essential for defining the genotoxic potential of the compound. The aim of this study was to develop a simple UHPLC method coupled with tandem mass spectrometry (MS/MS) for chemical characterization of an unknown degradant, and the separation and quantification of ziprasidone and its five main impurities (I–V) in the raw material and pharmaceuticals. Chromatographic conditions were optimized by experimental design. The MS/MS fragmentation conditions were optimized individually for each compound in order to obtain both specific fragments and high signal intensity. A rapid and sensitive UHPLC–MS/MS method was developed. All seven analytes were eluted within the 7 min run time. The best separation was obtained on the Acquity UPLC BEH C₁₈ (50 × 2.1 mm × 1.7 μm) column in gradient mode with ammonium‐formate buffer (10 mm ; pH 4.7) and acetonitrile as mobile phase, with the flow rate of 0.3 mL min^?1 and at the column temperature of 30°C. The new UHPLC–MS/MS method was fully validated and all validation parameters were confirmed. The fragmentation pathways and chemical characterization of an unknown degradant were proposed and it was confirmed that there are no structural alerts concerning genotoxicity.