多波长K系数法测定氯芬待因复方片剂的含量

本文报道了多波长Ｋ系数法测定氯芬待因复方片剂中双氯芬酸钠、磷酸可待因两组分含量的研究。结果表明,双氯芬酸钠在１１．１８～２５．４０μｇ／ｍＬ、磷酸可待因在６．７８５～１５．４２μｇ／ｍＬ范围内ΔＡ值与浓度线性关系良好,回归方程分别为ΔＡ双＝－０．００６７４ｃ双－１．４１８５×１０－３,ｒ＝０．９９９６;ΔＡ＝－０．０１３０ｃ可－１．８２２×１０－３,ｒ＝０．９９９８。双氯芬酸钠和磷酸可待因的平均回收率及相对标准偏差分别为１００．１％,０．３６％;１００．７％,０．８０％。方法简便,快速,结果满意。     

P—矩阵法测定安钠咖注射液中两组分的含量

本文采用Ｐ－矩阵法不经分离同时测定安钠咖注射液中咖啡因和苯甲酸钠的含量。计算程序用ＢＡＳＩＣ语言编制。咖啡因和苯甲酸钠的平均回收率分别为１００．０和９９．９５％，变异系数分别为０．４０％和０．６５％，方法简便，快速，样品测定结果与药典法测得结果基本一致。     

ICP－AES法测定铂催化网中的次成分及杂质元素

本文采用ＩＣＰ－ＡＥＳ内标法，对硝酸生产用铂催化剂的次成分Ｐｄ和Ｒｈ，以及十一个杂质元素，进行直接快速测定。部分受干扰的元素，采用扣除其相应等效强度的方法进行校正。本方法的回收率和相对标准偏差，对于次成分分别为：９９．１～１００％和０．１６～０．３１％；对于杂质元素分别为：９５～１１４％和０．８３～１３％。     

ICP—AES法测定铂催化网中的次成分及杂质元素

本文采用ＩＣＰ－ＡＥＳ内标法，对硝酸生产用铂催化剂的次成分Ｐｄ和Ｒｈ，以及十一个杂质元素，进行直接快速测定。部分受于扰的元素，采用扣除其相应等效强度的方法进行校正。本方法的回收率和相对标准偏差，对于次成分分别为：９９．１～１００％和０．１６～０．３１％，对于杂质元素分别为：９５～１１４％和０．８３～１３％。     

FAAS 测定铜对 CaS DCEL粉末包铜工艺的指导

利用火焰原子吸收光谱法（ＦＡＡＳ），建立了以ＣａＳ为基质的粉末发光材料，包铜量的定量分析方法，回收率和相对标准偏差分别为９９．４￣１００．６与０．４％。在准确度满足工艺要求的情况下，通过是到的测试数据及曲线，给出了在包铜过程中，包铜液的浓度，温度，时间等参数对包铜量的影响，进行了操作模式，使材料的性能得到了提高。     

碳酸锶共沉淀富集火焰原子吸收法测定微量镉

用碳酸锶作为载体共沉淀富集镉使火焰原子吸收法测定镉的灵敏度大幅度提高。特征浓度０．０４４μｇ·ｍｌ－１／１％，加标回收率９９．７５～１０４．５％，ＳＤ是０．００６，ＣＶＳ．５２％。     

镧对镝-磺基水杨酸配合物荧光增强效应的研究和应用

本文研究发现,三价稀土离子Ｌａ３＋的存在对二元配合物Ｄｙ３＋－磺基水杨酸（ＳＳＡ）体系具有强烈的荧光增强效应。在常温条件下,研究了Ｌａ３＋参与下Ｄｙ３＋－ＳＳＡ体系的荧光特性、形成条件和影响因素,结果表明,Ｌａ３＋可使Ｄｙ３＋－ＳＳＡ体系荧光增强１００倍。在最佳条件下,Ｄｙ的浓度在３．０×１０－７～１．０×１０－５ｍｏｌ／ｄｍ３范围内与荧光强度成线性关系,检测限达到８．０×１０－８ｍｏｌ／ｄｍ３。利用该体系测定了合成稀土样品和包头稀土标准样品,结果满意,回收实验的回收率为９９．３％±０．１％。     

“天光”一号MOPA系统光学元件加工与镀膜的进展

本文阐述了在中国原子能科学研究院“天光一号”ＫｒＦ激光核聚变实验装置上，ＭＯＰＡ系统光学元件加工与镀膜研究工作的进展。实验测量结果表明，加工后的基片表面均方根粗糙度对于Ｋ９光学玻璃与熔融石英玻璃来说分别为σｒｍｓ＝１．８±０．５ｎｍ，σｒｍｓ＝２．０±０．４ｎｍ。镀ＨｆＯ２／ＳｉＯ２高反射膜的光学元件的反射率与破坏阈值分别为Ｒ＞９９．５％，Ｅｔｈ＝１．３０～１．３３Ｊ／ｃｍ２。镀Ａｌ２Ｏ３／ＭｇＦ２增透膜的光学元件的透射率与破坏阈值分别为Ｔ＞９９．５％，Ｅｔｈ＝１．３～１．９７Ｊ／ｃｍ２。     

钼盐涂覆－塞曼无火焰原子吸收法测定肿瘤患者血清中的微量镍

用钼盐涂覆石墨管，使ＧＦＡＡＳ测镍灵敏度大幅度提高，加入偏钒酸铵和镧为基体改进剂，消除干扰，特征质量为２４．８４ｐｇ／０．００４４Ａ．Ｓ．加标回收率９４．９７～１１１．１５％。标准偏差０．０３０９，ＣＶ８．１３％。     

钼盐涂覆—塞曼无火焰原子吸收法测定肿瘤患者血清的微量镍

用钼盐涂覆石墨管，使ＧＦＡＡＳ测镍灵敏度大幅度提高，加入偏钒酸铵和镧为基体改进剂，消除干扰，特征质量为２４．８４ｐｇ／０．００４４Ａ．Ｓ．加标加收率９４．９７～１１１．１５％。标准偏差０．０３０９，ＣＶ８．１３％。     

PMR Assay of Natural Products in Pharmaceuticals. IV Assay of Codeine and Simultaneous Detection of Morphine

A rapid, accurate and precise PMR method is presented for the quantitative determination of codeine and codeine phosphate as bulk drugs and in tablet dosage form. The determination is based on the integration of the C-3 methylprotons or the two aromatic protons of codeine or its salt relative to that of the nine protons of t-butanol. Standard deviations of ± 1.39, 0.27 and 0.65% were obtained for codeine, codeine phosphate bulk drug and codeine phosphate tablets respectively. The method furnishes a specific means of identification of codeine as well as of the simultaneous detection and possible determination of morphine; thus fulfilling one of the most important pharmacopeial requirements for the purity of codeine.     

近红外高光谱成像技术在筛查保健食品中违禁添加抗炎药物双氯芬酸钠的研究

双氯芬酸钠是一种非甾体抗炎药,抗炎症效果较好,抗炎化学药物双氯芬酸钠有可能违禁添加到缓解炎症保健食品中.目前已有一些文献研究水、肉及牛奶等中的药物双氯芬酸钠,主要利用高效液相色谱、表面增强拉曼及电化学等方法,需要相对复杂的预处理过程,操作步骤相对复杂,耗时.为了快速、无损检测保健食品中违禁添加物的成分,探索建立采用10...     

荷移分光光度法测定可待因

采用分光光度法研究了电子受体7,7,8,8-四氰基对苯醌(TCNQ)与电子供体可待因的荷移反应, 发现TCNQ与可待因在丙酮介质中易发生荷移反应,并生成稳定的络合物,药物的最大的吸收峰由紫外区移至近红外区。据此建立了一种测定药物制剂中可待因含量的高选择性的荷移分光光度法,在最佳条件下,可待因浓度在0.1～1.6 μg·mL-1范围内符合朗伯-比尔定律,在最大吸收波长845 nm处,表观摩尔吸光系数为1.7×104 L·mol-1·cm-1。文章还研究了缔合常数和自由能变化并探讨了荷移反应的机理。该方法已用于片剂中可待因含量的测定,其回收率为(98.94±0.96)%～(99.12±1.21)%。     

Degradation of diclofenac sodium using combined processes based on hydrodynamic cavitation and heterogeneous photocatalysis

Diclofenac sodium, a widely detected pharmaceutical drug in wastewater samples, has been selected as a model pollutant for degradation using novel combined approach of hydrodynamic cavitation and heterogeneous photocatalysis. A slit venturi has been used as cavitating device in the hydrodynamic cavitation reactor. The effect of various operating parameters such as inlet fluid pressure (2–4 bar) and initial pH of the solution (4–7.5) on the extent of degradation have been studied. The maximum extent of degradation of diclofenac sodium was obtained at inlet fluid pressure of 3 bar and initial pH as 4 using hydrodynamic cavitation alone. The loadings of TiO₂ and H₂O₂ have been optimised to maximise the extent of degradation of diclofenac sodium. Kinetic study revealed that the degradation of diclofenac sodium fitted first order kinetics over the selected range of operating protocols. It has been observed that combination of hydrodynamic cavitation with UV, UV/TiO₂ and UV/TiO₂/H₂O₂ results in enhanced extents of degradation as compared to the individual schemes. The maximum extent of degradation as 95% with 76% reduction in TOC has been observed using hydrodynamic cavitation in conjunction with UV/TiO₂/H₂O₂ under the optimised operating conditions. The diclofenac sodium degradation byproducts have been identified using LC/MS analysis.     

Effects and mechanism of diclofenac degradation in aqueous solution by US/Zn0

A system of ultrasound radiation coupled with Zn⁰ was applied to degrade diclofenac. The effects of initial pH, dosage of Zn⁰ and ultrasound density were investigated. To further explore the mechanism of the microcosmic reaction, the fresh and used Zn⁰ powders were characterized by SEM, XRD and XPS. Radical scavengers were used to determine the oxidation performance of strong oxidizing free radicals on diclofenac, including hydroxyl radicals and superoxide radicals. The results showed that the optimum removal of diclofenac reached to over 85% at pH of 2.0 in 15 min, with Zn⁰ dosage of 0.1 g/L and ultrasound density of 0.6 W/cm³. TOC removal of 72.6% in 15 min and dechlorination efficiency of diclofenac reached 70% in 30 min. Characterization results showed that a ZnO membrane was generated on the surface of Zn particles after use. According to the mass spectrometry results, several possible pathways of diclofenac degradation were proposed, and most diclofenac was turned into micro-molecules or CO₂ finally. The synergistic effect of US/Zn⁰ in the reactions led to a proposed degradation mechanism in which zinc could directly attack the target contaminant diclofenac because of its good reducibility with the auxiliary functions of ultrasonic irradiation, mechanical shearing and free radical oxidation.     

发射光谱法测定高纯银中微量金、铂、钯、铑、铱、锑、铅、铋、铁、铜、镍、铬、铝和锌

本文研究了贵金属标准溶液除氯离子的有关问题，解决了高纯硝酸银中贵金属等杂质元素的标样配制，以硝酸银直接压样于普通电极中直流电弧激发，可测定９９．０～９９．９９％的高纯银，该方法简便、快速、准确。     

Plate-like hydroxyapatite nanoparticles synthesized by the hydrothermal method

In this article, calcium nitrate (Ca(NO₃)₂) and disodium hydrogen phosphate (Na₂HPO₄) are used as calcium and phosphorous sources to prepare hydroxyapatite nanoparticles by the hydrothermal method. Plate-like nanocrystals of hydroxyapatite are synthesized with the aid of sodium tripolyphosphate. The results show that sodium tripolyphosphate increases the diameters of the hydroxyapatite nanoparticles during the hydrothermal process. When the concentration of sodium tripolyphosphate reaches 0.015 M, the average aspect ratio of those nanoparticles is close to 1. The strong surface adsorption caused by sodium tripolyphosphate may answer for the morphological change of hydroxyapatite crystal.