高效液相色谱在药物毒物分析中的应用进展

本文综述了近几年新型高效液相色谱(HPLC)仪器及其部件的研制、发展以及在药物毒物分析中的应用进展概况。对于高效液相色谱仪中的一些新型检测器如二极管阵列紫外检测器,红外检测器,核磁共振检测器,质谱检测器,蒸发光散射检测器及激光小角度散射检测器等的研制与发展进行了阐述。对于高效液相色谱新技术及其制剂分析、在中草药及其制剂分析、在临床体液中分析、在毒物分析方面的应用进展进行了论述。     

蒸发光散射检测器计量性能验证

0引言蒸发光散射检测器（Evaporative Light-Scattering Detector,简称：ELSD）是一种新型的通用型质量检测器,不同于紫外或荧光检测器,ELSD的响应不依赖于物质的光学特征,任何挥发性低于流动相的物质均可以被检测。     

HPLC-ELSD法测定普瑞巴林的光学纯度

目的:建立高效液相色谱-蒸发光散射检测法(HPLC-ELSD)检测普瑞巴林的光学纯度。方法:选择ChiralcelOD-H色谱柱(250mm×4.6mm);以正己烷-异丙醇-三氟乙酸(965:32:3)为流动相;流速为0.5mL/min;采用蒸发光散射检测器,漂移管温度为80℃,载气流速为1.6L/min。结果:普瑞巴林的两种光学异构体(S/R)达到良好分离,R-异构体在1.013～10.13μg/mL范围内线性良好,r=0.99902,平均回收率为99.6%(n=15),检测限为12.3ng。结论:本文建立方法简单、快速、灵敏、准确、可靠,适用于普瑞巴林及制剂的光学纯度检测。     

黄杨宁滴丸的高效液相色谱——蒸发光散射检测器含量测定方法

目的:建立黄杨宁滴丸的高效液相色谱蒸发光散射检测器的含量测定方法。方法:通过交试验的建立,摸索影响蒸发光散射检测器性能的四个重要参数(漂移管温度,雾化气体流量,流动相流速,撞击器位置)的最佳搭配。结果:黄杨宁滴丸含量采用HPLC(ELSD)测定,经方法学研究结果表明,方法准确可靠、灵敏度高、重现性好,可以作为黄杨宁滴丸中环维黄杨星D的定量分析方法。而且较原质量标准含量测定法中酸性染料法步骤简单,重现性好,检验周期尽需半天。     

用于气体分析的气相色谱技术

本文从色谱柱、检测器、如何减小峰形拖尾、如何选择定值方法等四个方面,论述了气相色谱在气体分析中的应用技术。     

烟用香精香料的高效液相色谱-蒸发光散射法质量控制研究

为了监控烟用香精香料的质量,应用高效液相色谱-蒸发光散射仪,Nova-Pak C18柱(4μm,150mm×3.9mm),以烟酸甲酯为内标,乙醇-水(71:29)为流动相,等度洗脱,流速1.0mL/min,对烟用香精香料进行HPLC分析,通过对待测样品与标准样品的指纹图谱谱峰匹配,计算指纹图谱间的相似度考察烟用香精香料质量稳定性。     

JJG705-2014《液相色谱仪检定规程》修订说明

<正>一、修订背景《液相色谱仪检定规程》最早制定于1990年,2002年进行了第一次修订,主要增加了当时应用较多且较成熟的二极管阵列检测器的检定内容。随着科学仪器的不断进步与发展,液相色谱仪的检测器不断地被开发应用,以满足分析科学的发展需求。其中应用发展比较快的是蒸发光散射检测器。蒸发光散射检测器是基于被分析物的散射机理检测的,即色谱柱中流出物被高速氮气喷成雾状液滴,溶剂挥发后形成微小颗粒,被载气带到散射室,检测其散射光强度。比流动相挥发性小的物质都能被检测,是通用型检测器。对于     

液相色谱仪最小检测浓度测量值的不确定度评定

本文介绍了2014年8月14开始实施的JJG705-2014《液相色谱仪检定规程》中涉及的液相色谱仪紫外-可见检测器、二极管阵列检测器、荧光检测器、示差折光率检测器、蒸发光散射检测器最小检测浓度测量不确定的评定方法。     

液相色谱仪－蒸发光散射检测器的检定

本文详细描述了按照新版JJG 705—2014液相色谱仪检定规程的要求,对液相色谱仪－蒸发光散射检测器进行检定的过程,并总结了检定过程中的经验和注意事项,以供广大检定员参考。     

火箭推进剂液氢中氦的分析方法

使用气相色谱法分析氢中氦时,在常用色谱柱上氦出峰在氢后面,并且位置很近,较大的氢峰会掩盖氦峰。针对上述问题,研制了一种新的色谱柱固定相,用于色谱法分析氢中氦组分。给出了这种固定相对氢、氦组分的分离原理、制作方法和实验过程。实验结果表明,采用气相色谱热导检测器,配用金属钯做色谱柱固定相,可成功地完成对氢、氦组分的分离和检测。     

Selective detection of volatile aromatic compounds using a compact laser ionization detector with fast gas chromatography

We report results for a new gas chromatography detector that is comparatively sensitive and far more selective for aromatic compounds than the traditional photoionization detector. The detection means is multiphoton ionization at atmospheric pressure. The ionization source in these experiments is a diode-pumped passively Q-switched microchip laser operating at 266 nm. Experiments were conducted with the detector interfaced to a fast gas chromatograph. For <20 s elution time, limits of detection were <1 pg for toluene, ethylbenzene, xylenes, and isopropylbenzene; the limit of detection for benzene is approximately 10 pg. Detector response was linear over 5 orders of magnitude, including these low levels. Negligible signals were observed for nonaromatic ketones, aldehydes, ethers, and cycloalkanes at levels as high as 0.1 microg (10 mg/L concentration). Detector efficiency after fast GC separation was 0.002% when using a detector cell with a radius of 1.1 cm and a purge gas flow of 500 mL/min. The advantages of this detector are further illustrated by the fast GC analysis of fuel samples.     

一种计算机层析成像用X光高分辨探测器技术

探测器技术是计算机层析成像系统的关键技术之一。提出了一种基于面阵CCD器件,采用 光纤和光纤面板进行光耦合及传输的扇形束线阵扫描X射线新型探测器技术。实验结果表明,该新型探测器具有结构紧凑、性能可靠且分辨力高(约50μm)等特点,可以实际应用于工业X-CT系统之中。     

White light emission from spin coated Gd2O3:Dy nano phosphors synthesized using polyol technique

Water dispersible Gd2O3:Dy3+ (2%) nanophosphors were synthesized through a facile polyol process and characterized by using X-ray diffraction (XRD), transmission electron microscopy (TEM), Dynamic Light Scattering (DLS) and photoluminescence (PL) spectrophotometry. The results of XRD, TEM and DLS show that resultant nanoparticles are single phasic and have spherical shape with 17 to 22% dispersibility. An efficient energy transfer was observed from host to the dopant ions. Characteristic blue and yellow emissions from Dy3+ ions were observed. The CIE coordinates of the nanophosphor lie in the white light region of the chromaticity diagram. Spin coating of the nanophosphor was done on quartz substrate. Bright white luminescence of this film was observed under ultraviolet light with lamda exc = 310 nm.     

氩放电检测器气相色谱仪在高纯氩气检测中的应用

氩放电检测器(Argon Discharge Detector)是一种用氩气做载气的气相色谱仪专用检测器,因其具有独特的检测能力,在氩气检测领域应用较为广泛。采用AGC仪器公司生产的Nova CHROM2000搭载氩放电检测器(ADD)气相色谱仪,对该检测器的检测能力进行评测。     

Response function of a beta detector telescope consisting of HPGe and scintillator

The response function of a beta detector telescope consisting of a 15 mm thick high purity germanium detector stacked with a 1 mm thick plastic scintillation detector has been determined. The telescope covers the energy range from 1 to 14 MeV. Detector response and relative efficiencies were measured at four electron energies between 2.5 and 8.5 MeV. The monoenergetic electrons were obtained using conversion electrons originating from thermal neutron capture in a ¹¹³Cd target.     

氦离子色谱仪在四氟化碳分析中的应用

采用氦离子检测器（PDHID）及以热导检测器（TCD）与火焰离子化检测器（FID）组合的两种不同气相色谱分析方法测定四氟化碳（CF4）中的杂质,结果表明氦离子化检测器（PDHID）灵敏度更高,检测限更低,更适用于电子气体CF4的检测。     

Measurements of detector nonlinearity at 193 nm

We have developed a measurement system based on a correlation method to characterize the nonlinearity of a detector's response over a large range of laser pulse energy. The system consists of an excimer-laser source, beam-shaping optics, a beam splitter, a monitor detector, a set of optical filters, and the detector under test. Detector nonlinearities as large as 10% or greater over an entire measurement range at an excimer-laser wavelength of 193 nm are observed. The measurement range of the current system is approximately 300 nJ to 50 mJ of laser pulse energy at the detector under test. The typical expanded measurement uncertainty of nonlinearity is 0.6% (k = 2).     

A phoswich detector for high-energy neutrons

A phoswich detector was developed to measure neutron energy spectra from a few MeV to a few hundreds MeV in aircrafts and space crafts. Radiation fields, which both crafts are exposured, consist of neutrons, gamma rays, protons, etc. The phoswich detector can measure neutrons separately from gamma rays and protons. The capability of particle discrimination was tested at HIMAC and was found to be excellent. Detector response functions to neutrons were simulated with the MCNPX code using the measured light outputs of charged particles and were measured with quasi-mono-energetic neutrons produced by the p-Li reaction at the NIRS cyclotron. Test flight measurements at high altitudes, 6.5 and 8.5 km, were performed above the middle part of Japan (cut-off rigidity, 12 GV).     

Characterization of an Al-STJ-based X-ray detector with monochromatized synchrotron radiation

The characterization of an Al-STJ-based detector with Pb absorber was performed with monochromatized synchrotron radiation. Detector response was measured in the energy range from 3 to 10 keV. A small non-linearity of the signal pulse height was detected, probably due to the escape of recombination phonons from the detector. The non-linearity can be described by a second order polynomial function. Additionally, detector signals were recorded while an X-ray beam of 50 μm diameter was directed to several locations on and near the absorber. For a well-aligned beam, detector artefacts are of at least two orders of magnitude lower intensity than the absorber events.     

Chevron detector design study

Results obtained in a design study which has attempted to optimize the detector chevron and interconneetion geometry are reported. The detector waveform with interconnections between chevrons placed at alternating ends of the chevrons is redundant, with the second half cycle largely repetitious of the first as the domain traverses the detector. The present designs attempt to select the first half cycle by placing the second set of interconnections asymmetrically, near the center of the chevron column. The selected signals are then enhanced by narrowing the chevron linewidth on the incoming side where the serpentine current path is defined. Detector waveforms obtained with such designs have a high resistance state, when a bubble is present, which peaks just before a rapid change into a low resistance state such that the maximum excursion can be used with conventional clamp and strobe sense amplifiers. The dependence of the output on linewidth, garnet thickness, and static in-plane offset field are investigated experimentally. Detector figures of merit, i.e., signal voltage divided by dc voltage, of 0.5% have been observed and appear robe obtainable in a practical sense.