气相色谱法快速测定蚊香及蚊香原料中丙烯菊酯

丙烯菊酯是蚊香的活性组分。关于蚊香中丙烯菊酯的测定报道甚少。文献中[1]采用电子俘获检测器检测,线性关系差,检测器易污染。文献[2]中采用振摇提取,操作繁琐。本法采用甲醇超声提取,气相色谱分离,FID检测操作简单,快速,准确。     

气相色谱法快速测定家用气雾杀虫剂中丙烯菊酯、氯菊酯、增效醚含量

用气相色谱法定量测定了家用气雾杀虫剂中的丙烯菊酯、氯菊酯和增效醚。色谱柱为５％ＱＦ－１／Ｃｈｒｏ－ｍｏｓｏｒｂＷＨＰ,以邻苯二甲酸二苯酯为内标物,测得的回收率分别为１００％,１０２％,９９．９％;变异系数为０．１３,０．５６,０．４８,方法简便、快速、准确。     

毛细管气相色谱法测定电热蚊香液中的丙炔菊酯

采用HP－1毛细管气相色谱法对电热蚊香液中丙炔菊酯的含量进行了定量分析，其测定结果的相对标准偏差为0．3％，回收率为103．05，具 有操作准确、简便，快速和实用等特点。     

二阶导数极谱法同时测定氯菊酯和生物丙烯菊酯及其电极过程研究

本文对氯菊酯的极谱行为进行了研究,发现在pH1.1乙醇-B.R缓冲溶液中-1.25V处氯菊酯有一还原峰,在-1.04V处生物丙烯菊酯有一还原峰。其线性范围分别为8×10~(-6)～6×10~(-5)g/ml和4×10~(-7)～6×10~(-5)g/ml。氯菊酯的极谱波系吸附控制的还原波,电子转移数为2。应用本法对氯菊酯,生物丙烯菊酯进行同时测定,结果令人满意。回收率为97.2％～105.5％。     

气相色谱法测定喷雾杀虫剂中的胺菊酯和氯菊酯

用SE-30毛细管柱、160~300℃程序升温、以邻苯二甲酸二环己酯为内标物,气相色谱法同时测定家用气雾杀虫剂中有效成分胺菊酯、氯菊酯的含量。胺菊酯、氯菊酯的平均回收率分别为94.0%、95.4%,相对标准偏差分别为2.23%、6.73%。     

生物丙烯菊酯在手性柱上的拆分

1　引　　言生物丙烯菊酯是一种高效、低毒的杀虫剂 ,化学名为 (ＲＳ) 3 烯丙基 2 甲基 4 氧代环戊 2 烯基 (1Ｒ ,3Ｒ) 2 ,2二甲基 3 (2 甲基丙 1 烯基 )环丙烷羧酸酯。曾有报道 ,在 β 环糊精衍生物、ＰｉｒｋｌｅＩ Ａ离子型等手性固定相上对丙烯菊酯进行了拆分。本文利用自制的手性固定相ＣＤＭＰＣ、ＣＭＰＣ对生物丙烯菊酯进行了手性拆分 ,并优化了流动相的组成。2　实验部分2 .1　试剂　ＣＤＭＰＣ、ＣＭＰＣ结构分别为纤维素 3(3,5 二甲基苯基氨基甲酸酯 )、纤维素 3(4 甲基苯基氨基甲酸酯 )。球形硅胶 (中国科学院兰州…     

凝胶渗透色谱-固相萃取净化测定茶叶中16种菊酯残留量

建立了以凝胶渗透色谱(GPC)和固相萃取(SPE)净化,气相色谱-质谱(GC-MS)负化学源(NCI)技术测定茶叶中七氟菊酯、 四氟菊酯、丙烯菊酯、联苯菊酯、胺菊酯、甲氰菊酯、氯氟氰菊酯、氟丙菊酯、苯醚氰菊酯、氟氯氰菊酯、氯氰菊酯、氟氰戊菊酯、氰戊菊酯、 氟胺氰菊酯、溴氰菊酯、氯菊酯等16种菊酯残留量的方法.样品经V(丙酮)∶V(乙酸乙酯)∶V(正己烷)＝1∶2∶1提取,经GPC去除大分子的色素和类脂杂质,弗罗里硅土 SPE柱进一步净化,以毒死蜱同位素D-10作内标,内标法定量.方法的回收率67.2%～108%之间.变异系数小于18%.16种菊酯方法定量限在0.0125～0.025 mg/kg之间.     

氯菊酯胺菊酯混合防蛀剂的气相色谱法测定

用３％ＯＶ－１０１２ｍ×３ｍｍｉ．ｄ．玻璃或不锈钢柱,以邻苯二甲酸二（２－乙基）己酯为内标,在柱温２２３℃时同时测定氯菊酯胺菊酯混合防蛀剂中有效成分——氯菊酯和胺菊酯的质量分数。方法中氯菊酯和胺菊酯的平均变异系数分别为０．２０％和０．１９％。     

新型含异恶唑环醚菊酯的合成（I）

拟除虫菊酯是一类在研究除虫菊素化学结构和药效的基础上发展起来的新型农药,而80年代后期开发的醚菊酯,除具备拟除虫菊酯杀虫谱广、稳定性强、药效高以外,另一个显著的特点是对温血动物低毒.而异唑衍生物有涉及杀虫、杀菌、除草的多种活性[1-3],将其引入醚菊酯的结构中有望得到理想活性的化合物.为此,以各种芳香醛通过氧化腈和溴丙炔的偶合加成制备异唑衍生物,然后和2-取代苯基-2-甲基-丙醇反应,制得22个醚菊酯类新化合物,并且通过了红外光谱、核磁共振、质谱或元素分析的结构鉴定.     

0.3%胺菊酯·右旋苯醚菊酯气雾剂的高效液相色谱分析

提出了采用高效液相色谱法,使用Hypersil C18不锈钢色谱柱和乙腈-水(85+15)混合溶液为流动相进行分离,并用紫外检测器在220 nm波长处同时测定胺菊酯和右旋苯醚菊酯,此方法用作上述两杀虫剂的复合制剂0.3%胺菊酯.右旋苯醚菊酯气雾剂的质量监控分析方法。测得两化合物的相对标准偏差(n=5)依次为0.86%和2.6%,回收率依次在94.7%~105.5%和92.8%~102.9%之间。     

A stability-indicating reversed-phase high performance liquid chromatography method for simultaneous assay of two corticosteroids and estimation of their related compounds in a pharmaceutical injectable formulation

Betamethasone Sodium Phosphate and Betamethasone Acetate are the two corticosteroids active pharmaceutical ingredients (APIs) that are present in the injectable formulation, Celestone Chronodose^® Injection. It is extremely challenging to develop a Quality Control friendly HPLC method to separate all the potential impurities and degradation products of the two APIs from each other using a single HPLC method. A novel stability-indicating reversed-phase HPLC (RP-HPLC) method using two oxo-cyclic organic modifiers in the mobile phase was developed and validated. This method can separate a total of 32 potential impurities and degradation products from the two APIs and also from each other. Peak symmetry and separation efficiency were enhanced by using two chaotropic agents (trifluoroacetic acid and potassium hexafluorophosphate) in the mobile phases of this method. The stability-indicating capability of this method has been demonstrated by analyzing aged and stressed degraded stability samples of the drug product. This method uses an ACE 3 C18 (15 cm × 4.6 mm) HPLC column. The method was validated per ICH guidelines and proved to be suitable for routine QC use.     

乘子罚函数分光光度法测定安钠咖注射液的含量

本文报道将乘子罚函数法用于处理多波长吸光度数据,同时测定样品中多组分的含量。简要介绍了原理和计算步骤。对安钠咖注射液模拟样和实际样品中的咖啡因、苯甲酸钠进行了测定,１２份模拟样中咖啡因和苯甲酸钠的回收率分别为（１００．１６±０．５４）％和（９９．７４±０．３４）％（置信度９５％）,实际样品分析的结果与药典法一致。     

A two‐step method for rapid characterization of electroosmotic flows in capillary electrophoresis

The measurement of electroosmotic flow (EOF) is important in a capillary electrophoresis (CE) experiment in terms of performance optimization and stability improvement. Although several methods exist, there are demanding needs to accurately characterize ultra‐low electroosmotic flow rates (EOF rates), such as in coated capillaries used in protein separations. In this work, a new method, called the two‐step method, was developed to accurately and rapidly measure EOF rates in a capillary, especially for measuring the ultra‐low EOF rates in coated capillaries. In this two‐step method, the EOF rates were calculated by measuring the migration time difference of a neutral marker in two consecutive experiments, in which a pressure driven was introduced to accelerate the migration and the DC voltage was reversed to switch the EOF direction. Uncoated capillaries were first characterized by both this two‐step method and a conventional method to confirm the validity of this new method. Then this new method was applied in the study of coated capillaries. Results show that this new method is not only fast in speed, but also better in accuracy.     

两种拔尿管方法对膀胱功能损伤的临床观察

为观察两种不同的拔尿管方法对膀胱功能损伤的差异,将80例患者随机分成两组,分别采用改良法(40例)和常规法(40例)拔除留置尿管,分析比较了两组患者排尿顺利率、逼尿肌功能恢复率及尿道刺激症、尿失禁、尿潴留。结果表明,两组患者拔管后上述指标与情况有显著性差异,P<0.05。提示改良组膀胱功能损伤明显低于对照组。改良的拔管方法是一种值得护理推广应用的好方法。     

测定两干扰组分体系的新的吸光度图解法——定组分比推论法的研究

吸光光度法是广泛应用的一种方法,但在待测溶液中如果存在严重干扰的元素,方法将失效。本文试图从理论上研究出一种新的图解法.提出了测定两干扰组分体系的吸光度图解法--定组分比推论法。应用该法使用通常的分光光度计,不经分离或掩蔽,能在一种严重干扰元素存在下顺利地测定欲测元素的含量。本文从理论上研究了定组分比推论法的原理,并通过实验给以验证。它具有一定的普遍性,运用这种推理的方法,有可能扩大到其他领域。由于方法原理简单、无需特殊的仪器,故易于推广应用。     

Preparation of Porous Alumina Film on Aluminum Substrate by Anodization in Oxalic Acid

Self-ordering of the cell arrangement of the anodic porous alumina was preared in oxalic acid solution at a constant porential of 40V and a temperature of 20℃. The honeycomb structure made by one step anodization method and two step anodization method is different. Pores in the alumina film prepared by two step anodization method were more ordered than those by one step anodization method.     

A method for creating a non-equilibrium NT(P1-P2) ensemble in molecular dynamics simulation

A method is proposed for creating a non-equilibrium ensemble with a constant number of molecules, constant temperature and constant pressures with different target values in two reservoirs [referred to as NT(P(1)-P(2)) ensemble] that are connected by a finite length nanopore. This method includes two steps. The first step places a partition between the two reservoirs and then creates a static pressure field and a proper system volume by using two self-adjusting plates on which two external forces/pressures with different target values are exerted. The second step removes the partition and the two self-adjusting plates and the pressure difference between the two reservoirs is maintained by a "pump" designed to simultaneously create a periodic boundary condition between the two reservoirs and supply the necessary force (work) to a subset of molecules for a steady state flow. To examine this method, several cases using liquid argon with a truncated and shift Lennard-Jones potential under different target pressures and pump sizes were studied. Results show that the method proposed in this paper works well. In addition, the method proposed in this paper was compared with the other external force field methods. The results show that as long as the external force is applied to a restricted set of molecules away from the channel a constant pressure difference between two reservoirs is maintained. The advantage of the algorithm proposed here also sets the absolute pressures with different target levels in two reservoirs instead of it being arbitrary. Studies show that the fluid flow rate or permeability through a nanopore depends not only on the pressure difference between two reservoirs, but also on the absolute pressures in two reservoirs.     

新型双通道卡尔费休微量水分测定仪的研制

基于卡尔费休微量水分测定的基本原理,结合当今两种基本卡尔费休水分测定的方法:库仑法和容量法,以MSP430F2617新型处理器芯片为核心设计了一种双通道同时在线测量的微量水分测定仪,实现了一个系统中集成两种测量方法,扩展了仪器使用的灵活性。文中阐述了仪器双通道的设计方案,部分硬件电路,精度保证措施以及对仪器精度和性能的验证方法。     

Anwendung der Pyknometrie zur Bestimmung der Grenzen der gegenseitigen Löslichkeiten zweier Stoffe im festen Zustand

A new method of determining the solubility limits of two solid substances in one another is based on pyenometry combined, with chemical analysis and X-ray crystallography. By this means it is possible, using two samples, to draw the equilibrium diagram between the two solid substances at any temperature. It is shown experimentally that in the case of the pseudobinary system US—UC the method yields exact results. Finally, the range and limitations of the method are studied.     

Determination of the kinetic parameters from non-isothermal measurements with a general temperature program

This paper deals with a new method for the evaluation of the kinetic parameters from thermogravimetric measurements with a general temperature program. The procedure assumes the use of a computer or calculator. In principle, it is an integral method with two variants. The kinetic parameters can be determined from a single and/or from two general temperature programs. This method is free of the shortcomings that the existing method has, i.e. the self-heating and/or self-cooling, resulting in errors in measurements and the limitation of the weight of sample. The two variants of the submitted method have been tested by evaluation of the experimental data of the thermal decomposition of CaCO₂.