两种重组抗CD20人源化单克隆抗体定量分析方法的比较及其在药代动力学研究中的应用

采用酶联免疫吸附分析(ELISA)与基于Wil2-S细胞的流式细胞术(FCA)两种方法对生物基质中的重组抗CD20人源化单克隆抗体(rh-anti-CD20zumab)进行定量分析,并对两种方法进行系统比较。方法学验证结果表明,两种方法均具有良好的特异性、精密度和准确度,但定量范围存在明显差异。ELISA法批内和批间精密度均小于19.5%,准确度为-18.2%~17.6%;FCA法批内和批间精密度均小于19.0%,准确度为-18.9%~18.4%。二者定量范围分别为0.04~5.0 mg/L和3.1~200 mg/L,ELISA法的灵敏度显著高于FCA法。利用两种方法测定猕猴静脉滴注rh-anti-CD20zumab后的血药浓度-时间变化并进行药代动力学(PK)分析。结果表明,在给定剂量下,通过两种方法获得的PK结果具有良好的一致性。FCA法是一种细胞表面抗原靶向性抗体类药物PK研究及药效动力学(PD)研究的快捷、理想的方法。     

新的脉冲进样AAS法测定“麻杏石甘汤”中的微量金属元素

本文研制了一种新的脉冲进样装置，用于火娄原子吸收分光光度法测定中药煎剂中的Ｃａ，Ｍｇ，Ｆｅ，Ｍｎ，Ｚｎ五种金属元素含量，实验表明，利用此种装置可以同时获得两种进样方式的分析结果，线性范围比常规法宽两倍，耗样量，精密度及分析速度均优于常规法。     

磁性微粒子化学发光免疫分析法测定人血清中雌三醇

利用化学发光免疫分析(chemiluminescence immunoassay, CLIA)高灵敏度和高特异性的特点, 将磁性微粒子应用于化学发光免疫分析中, 用两种不同的方法对人体血清内的雌三醇(E3)含量进行了测定. 磁性微粒子分别作为固相一抗包被材料和二抗分离剂参与反应. 两种方法检测雌三醇浓度的线形范围均为0.6～60 ng/mL. 其中, 固相一抗法的批内变异及批间变异系数分别小于11%和15%, 回收率为90%～116%, 健全性系数为0.9987. 二抗分离法的批内变异及批间变异系数分别小于8%和10%, 回收率为88%～118%, 健全性系数为0.9974. 两种方法分别与经典板式化学发光法对比, 检测人血清样本, 结果相关性较好, 且磁性微粒子法更为省时、简便, 适于推广应用.     

离子选择电极法和新氟试剂光度法测定空气中HF的比较

对离子选择电极法与新氟试剂光度法的特性指标进行了比对研究。结果表明,离子选择电极法检出限为0.01 mg/L,线性范围为0.04～1 900 mg/L,相对标准偏差为0.16%～0.30%,加标回收率为101%;新氟试剂光度法检出限为0.05 mg/L,线性范围为0.06～1.5 mg/L,相对标准偏差为1.05%～2.10%,加标回收率为105%。两种方法结果无显著性差异,但离子选择电极法与新氟试剂光度法相比,测定下限低,测定范围宽,精密度、准确度较高,因此选定离子选择电极法作为制定大气中氟化氢测定法国家标准的基础。     

原子吸收光谱法间接测定血清离子钙及应用

对火焰原子吸收光谱法(FAAS)间接测定血清离子钙的分析方法进行了研究。并和离子选择性电极法(ISE)进行了比较。对这两种方法用标准加入法进行一元线性回归分析,r=0.985。对两种方法进行t检验,t=0.442,P>0.05。FAAS间接法相对标准偏差小于2％,加标回收率为98.5％。并应用于老年痴呆患者血清离子钙的测定。     

电极法测定废水中氨氮

介绍了采用电极法测定废水中氨氮时,以吹气法代替蒸馏法对废水水样进行预处理,简化了水样预处理的程序,样品中氨氮的释出率可达90%,加标回收率在60%-98.8%之间。对两种废水样各分析8次,得出其RSD值均小于5%。按3倍标准偏差计算方法的检出限为0.008 mg.L-1。定量测定的最高值为350 mg.L-1。     

混合氯化石蜡中短链氯化石蜡定量分析方法的比较

分别采用总体响应因子校正法和多元线性回归法对混合氯化石蜡中短链氯化石蜡进行定量分析,结果表明:两种方法均能较好地排除中链氯化石蜡的干扰,从而提高了短链氯化石蜡的定量准确性;但是两种方法均对标准曲线的浓度范围存在一定的依赖性,在使用这两种方法进行定量分析时,应将样品稀释到标准曲线适用的浓度范围。另外,相对于总体响应因子校正法,多元线性回归法定量范围更广。     

电感耦合等离子体质谱（ICP-MS）法与氢化物发生-原子吸收光谱（HG-AAS）法测定土壤中硒含量的对比研究

基于氢化物发生器与原子吸收光谱联用(HG-AAS),测定土壤样品中硒的含量,并与电感耦合等离子体质谱(ICP-MS)法测定值进行了对比。在两种仪器的最佳工作条件下,测定土壤硒的含量,实验结果表明:ICP-MS法和HG-AAS法对土壤硒含量测定的线性范围分别为0.85~100.00μg/L和0.08~16.00μg/L,检出限分别为0.25μg/L和0.02μg/L,精密度分别为1.3%和2.1%;用加标回收实验和测定国家标准土壤样品(GSS-7)对这两种方法的准确性进行了验证,ICP-MS法和HG-AAS法的加标回收率分别为96.7%~99.4%和94.9%~99.5%,GSS-7标准土样的结果均在标准值范围内,说明这两种测定土壤中硒含量的方法是准确可靠的。HG-AAS法测定线性范围窄,部分样品需要稀释,而且氢化物发生系统是手动进样,导致操作复杂,分析周期长;ICP-MS法仪器测定快速,但是仪器昂贵。     

两种乳糖酶活力测定方法比较

邻硝基苯-β-D-吡喃半乳糖苷(ONPG)法和双糖酶法是常用的乳糖酶活力测定方法,本文对这两种方法的线性范围、检出限、精密度、准确度和稳定性进行了比较。 结果显示,ONPG法在线性范围、检出限、精密度以及稳定性方面均优于双糖酶法,但此种方法的重复性较差,需要进一步的优化。 对比这两种方法,可为乳糖酶活力测定方法的合理选取提供参考。     

ICP-OES法与石墨炉原子吸收法测定饮用水中重金属元素比较

通过对比电感耦合等离子体发射光谱法(ICP-OES)与石墨炉原子吸收法(AAS)测定水中重金属的检出限、重复性、加标回收率等实验,验证两种方法的准确性,从而为饮用水中重金属的测定提供可靠的方法。结果表明,石墨炉原子吸收法测定饮用水中砷、镉、铬、铅、汞、硒检出限均低于ICP-OES法,但ICP-OES法测定线性范围宽,重复性和加标回收率均优于石墨炉原子吸收法,分析速度快,操作便捷,结果满意,是目前饮用水中重金属的测定非常可靠的方法。     

Preparation of degradable polypropylene by an addition of poly(ethylene oxide) microcapsule containing TiO2 part II. Modification of calcium phosphate on the TiO2 surface and its effect

To prepare a novel photo-degradable polypropylene (PP) with a higher degradation rate, a PP composite containing a poly(ethylene oxide) (PEO)/modified TiO₂ microcapsule was prepared. The modification of the TiO₂ was performed by the synthesis of octacalcium phosphate intercalated with succinic acid ion (OCPC) under various Ca/P molar ratio conditions. It was found that the synthesis conditions of the Ca/P = 3.5 and 3.6 M ratios were suitable to prepare the OCPC. However, the microscopic composition on the TiO₂ surface was different between these Ca/P conditions and affected the PP photo-degradation rate in the PP/PEO/modified TiO₂ composite. It was found from the Fourier Transform Infrared (IR) and the tensile testing measurements that the existence of the OCPC covering material on the TiO₂ surface brought about the higher PP photo-degradation rate. The facilitation behavior of the degradation was due to the release of the acid species (succinic acid ion) from the OCPC in the degradation process. In addition, the higher coverage of the OCPC on the TiO₂ surface brought about an induction period for the degradation.     

Ce-Zr-Ba-O纳米材料的制备及其结构与性能研究

以金属硝酸盐为原料,分别采用高分子前驱体法、柠檬酸盐凝胶法制备了纳米级的Ce-Zr-Ba-O复合氧化物超细粒子,采用X-射线衍射(XRD)、透射电镜(TEM)、BET比表面测定、热重-差热(TG-DTA)技术对催化剂进行了表征,并考察了催化剂的CO氧化活性和热稳定性。实验结果表明,高分子前驱体法和柠檬酸盐凝胶法制备的催化剂粉体都达到了纳米级。两种方法中,高分子前驱体法所制得的催化剂的BET比表面达118.96m²·g^-1,CO氧化反应活性较高,同时该方法制得的催化剂分散性好,无团聚,经1000℃高温焙烧后仍基本无烧结、无团聚现象,具有较高的热稳定性。     

Preparation of hollow PPy (HPPy) microspheres via template methods with characterization of properties

Template-synthesis method was one of the important methods for the preparation of hollow microspheres. In present work, polystyrene (PS) microspheres were initially synthesized and effects of reaction conditions on the particle size and distribution of PS microspheres were studied. Then sulfonated PS (SPS) microspheres and spherical core (PS) /shell (polypyrrole, PPy) were synthesized by sulfonated and template method respectively. The method was that pyrrole (Py) on the surface of SPS microspheres were polymerized. Then PS (core)-PPy (shell) microspheres by dissolving PS inner core in N, N-Dimethylformamide (DMF), and hollow polypyrrole (HPPy) microspheres were obtained (Figure 1). Thereafter, HPPy microspheres were characterized by fourier transform infrared spectroscopy, X-ray diffraction, particle size analyzer, scanning electron microscope, thermal gravimetric analysis and KDY-4 four-probe resistance meter. The results showed that the size range of PS microspheres were 200～300 nm. HPPy microspheres have been successfully synthesized with good electrical conductivity and excellent thermal stability.     

A Comparison of Methods for the Determination of Isocyanates in Air

Abstract

Isocyanates are in widespread use in certain industries such as in the manufacture of polyurethane products, paints and elastomers. The occupational exposure limit for isocyanates corresponds to 0.3 μg of isocyanate per sample using a 15 minute sampling time.

Airborne isocyanates cause a variety of respiratory problems and workplace monitoring is therefore necessary. Two methods have recently been published by the Health and Safety Executive, one colorimetric and one HPLC using both electrochemical and UV detection. This study has compared these two methods using both field samples and laboratory generated standard atmospheres over a range of concentrations relevant to test the method at occupational exposure levels. The result of the field study showed that the colorimetric method was generally being used at its limit of sensitivity. Although potentially more sensitive, HPLC did show some interference with the field samples, thus limiting its sensitivity. The laboratory study showed good correlation between the two methods down to below half the TLV.     

Preparation of degradable polypropylene by an addition of poly(ethylene oxide) microcapsule containing TiO2. Part III: Effect of existence of calcium phosphate on biodegradation behavior

In this work, biodegradation behavior of a novel polypropylene (PP) composite containing a poly(ethylene oxide) (PEO)/modified TiO₂ microcapsule was studied with an oxo-biodegradation test combined with a photodegradation treatment (using a high-pressure mercury vapor lamp for 24 h of the irradiation at 30 °C in air) and a soil burial test (for 45 days of incubation at 20 °C). The modification of the TiO₂ was performed by the synthesis of octacalcium phosphate intercalated with succinic acid ion (OCPC). The existence of the microcapsule brought about higher PP photo- and biodegradation rates. In the photodegraded PP composite, active colonies of some microorganisms were observed. By comparing with the PP composite without the OCPC modification, it was found that the active behavior of the microorganisms was due to the inorganic phosphates, which were supplied by the dissolution of the OCPC during the photodegradation. In addition, the photodegraded parts in the composite were completely metabolized by the microorganisms. However, the microorganisms had the inability to metabolize other parts such as the PP crystalline phase.     

电感耦合等离子体原子发射光谱法测定载钯树脂中钯的前处理方法考察

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定载钯树脂中的钯,对比了灰化法、硝酸-高氯酸法和微波消解法3种前处理方法,考察了称样量、消解加酸量、处理时间和灰化温度等对测定的影响,优化了最佳试验条件,讨论了共存离子的干扰.结果表明,钯质量浓度在0~50 mg/L范围内与强度线性关系良好,线性相关系数为0.999 5,灰化法、硝酸-高氯酸法和微波消解法3种方法的检出限分别为0.002 8、0.005 4、0.002 3 mg/L,相对标准偏差(n=11)分别0.69%、0.63%、0.42%,加标回收率分别为98%~100%、98%~101%、100%~104%.采用3种方法对实际样品进行测定,发现微波消解法处理时间最短,样品处理最完全,检测值最平行.用试验方法与原子吸收光谱法测定同一个载钯树脂,两者测定结果基本相符.     

超细钙钛矿复合氧化物的制备和性能研究

钙钛矿型复合氧化物(ABO_3)具有稳定的结构和较好的热稳定性,是一类被视为能够替代传统贵金属控制汽车尾气净化催化剂的新型三效催化剂。但其主要问题是比表面大小,一般小于10m~2·g~(-1),因此其催化活性的提高受到一定的限制。近几十年     

酒精度对高效液相色谱-荧光法分析白酒中氨基甲酸乙酯含量的影响

分析酒精度对高效液相色谱-荧光（HPLC-FLD）法测定白酒中氨基甲酸乙酯（EC）含量的影响,建立了快速检测白酒中EC含量的HPLC-FLD分析方法。通过比较不同酒精度下同一EC含量的峰面积,研究酒精度对EC含量测定的影响。结果表明,在5%~65%（v/v）酒精度范围内,酒精度与EC含量（峰面积）具有良好的线性关系,相关系数R²大于0.98,同时建立了不同酒精度间EC含量换算的相对校正系数。该方法在10~500 μg/L范围内呈良好的线性关系,R²大于0.9999,定量限为10 μg/L,加标回收率为98.9%~108.2%,相对标准偏差为0.6%~4.9%。评价了HPLC-FLD法的可靠性,将该方法与GC-MS方法比较,结果显示两种方法无明显差异。该方法简单、灵敏、准确,适用于白酒中EC含量的快速测定,具有较好的实际应用价值。     

亚硝酸根在纳米金修饰玻碳电极上的电催化氧化行为及其测定

采用直接电化学沉积法制备出纳米金修饰玻碳电极,研究了其对亚硝酸根的电催化氧化作用。结果表明,亚硝酸根在该修饰电极上于0.8 V处出现了一个良好的氧化峰。在最优实验条件下,亚硝酸根的峰电流与其浓度在2×10-6～2×10-3mol/L范围内呈一定的线性关系,检出限为6.0×10-7(S/N=3),提出了用循环伏安法测定亚硝酸根的方法。纳米金修饰电极用于东莞自来水水样中亚硝酸根的测定,回收率在98.1%～101.4%之间。对比本方法,用分光光度法对东莞自来水样中亚硝酸根进行了测定,结果满意。     

气相色谱-串联质谱法测定不同产地大米中的角鲨烯

通过比较大米中角鲨烯的不同提取方法,选用优化后的索氏提取/气相色谱-串联质谱(GC- MS/MS)法对不同产地大米中的角鲨烯进行定性及定量分析.结果表明,该方法在1-50 mg/L质量浓度范围内线性良好,相关系数为0.9987;检出限为0.1 mg/kg;在5,20 mg/kg 2个加标水平下的回收率可达96%-104...