矿物药大青盐中杂质元素的扫描电镜分析

目的通过对不同产地矿物药大青盐的扫描电镜分析研究,了解大青盐所含的杂质成分、杂质的含量及有害元素的组成。方法采用德国LEO1430VP环境扫描电子显微镜,配备INCA 200型X-射线能谱仪来分析大青盐。结果与结论通过扫描电镜能谱分析结果,大青盐主要含有氧、钠、镁、铝、硅、氯、钾、钙、铁、硫等元素,且不同盐中所含杂质差异较大;与大青盐伴生的化合物可能为钾、钙、镁、硅的氧化物,或含氧酸盐;也可能为钾、钙、镁的氯化物;同时也可能伴有钠的含氧酸盐。     

利用原子吸收法测定滑石粉中多种金属杂质的含量

目的：采用原子吸收法测定滑石粉中铅、铁、钙、铝等金属元素的含量。方法：利用原子吸收技术,采用标准曲线法进行滑石粉中金属杂质的测定。结果：所收集样品中金属杂质的含量均符合国外药典中滑石粉项下规定的限度要求。结论：该方法准确度高、重复性好,可用于滑石粉中金属杂质的含量测定。以确保滑石粉的安全使用。     

安徽省栽培玉竹中几种金属元素含量的测定

目的 了解不同地区栽培玉竹中金属元素含量的差异.方法 采用原子吸收分光光度法对安徽省栽培玉竹中的金属元素钾、钙、镁、锌、锰、铜、铁的含量进行测定.结果:各元素平均含量为:钾12.7047 mg/g,钙1.59083 mg/g,镁0.55495 mg/g,锌0.02034 mg/g,锰0.01839 mg/g,铜0.00664 mg/g,铁0.11791 mg/g,各元素组别间差异无统计学意义(P＞0.05).结论 栽培玉竹中钾、钙、镁、锰、铁含量受区域影响较大.     

滑石粉酸中可溶物过滤介质探讨

目的:研究不同过滤介质对滑石粉酸中可溶物测定结果的影响.方法:采用不同标准收载的过滤介质(中速滤纸和慢速滤纸),以及孔径为0.45μm的微孔滤膜对不同粒径与粒径分布的滑石粉酸中可溶物进行测定,并对测定结果进行分析比较.结果:采用不同孔径的过滤介质测定,酸中可溶物检测结果及结果的相对偏差随着过滤介质孔径减小而下降.结论:...     

滑石粉与石棉的微形态及元素构成的SEM/EDS微区分析

目的:进行滑石粉中主要元素的分析研究,并对滑石粉和石棉进行微形态分析。方法:利用扫描电子显微镜/X-射线能谱仪(Scanning Electron Microscope/Energy Dispersive X-ray Spectrometer)对滑石粉中元素组成进行了测定,计算它们的相对重量百分比,并进行滑石粉和石棉的微形态分析。结果:滑石粉中主要元素为Mg、Si,还有少量的Fe、Ca、Al等元素;石棉中也含有Mg、Si元素,但比例组成与滑石粉的比例组成不同。滑石粉中Si和Mg,二者相对重量百分比约为(1.3～1.7)︰1,温石棉样品中二者比约为0.6︰1。滑石粉的微区形态为致密块状或鳞片状,石棉的微区形态为长纤维状。结论:不同产地滑石粉中主要元素Mg、Si的比例基本相同。山东产的药用滑石粉中检出少量的Ca,而广西产的药用滑石粉中检出少量的Fe和Al,说明滑石粉中伴生元素的种类有地域特征;工业用滑石粉中均伴生有Ca、Fe和Mg。微形态分析能够直观区分滑石粉和石棉,为检测滑石粉中的石棉成分提供了新方法、新思路。     

影响药用辅料滑石粉白度的因素及关系分析

目的:研究影响药用辅料滑石粉白度的因素及其之间的关系分析。方法:首先对可能影响药用辅料滑石粉白度的因素(金属元素含量、粒度和粒度分布)进行测定，随后对测定结果进行主成分分析(PCA)推测主要因素，最后通过SPSS建立线性回归模型进行验证。结果:经PCA分析推测主要因素为杂质金属钙含量以及粒度D₉₀;建立的线性回归模型为：白度=96.457+42.770×钙%-0.422×D₉₀。其中R²为0.944,调整R²为0.934,P<0.05,模型构建有意义。结论:药用辅料滑石粉的白度由自身的杂质金属钙含量与粒度D₉₀共同影响，建立白度相关回归模型，为白度作为可视化量值用来控制滑石粉生产工艺与制剂中的粒度及杂质金属钙含量提供理论依据，也为药用辅料滑石粉的特性质量属性研究提供一种新思路。     

ICP-AES法同时测定碳酸锂原料药中6种杂质元素

目的：建立电感耦合等离子体发射光谱（ICP-AES)同时测定碳酸锂原料药中6种杂质元素（钙、钠、钾、镁、铁和铝）的分析方法,并分析不同厂商碳酸锂原料药的杂质含量。方法：用硝酸溶解样品, ICP-AES法分析样品中6种杂质元素的含量。结果：6种元素标准曲线的相关系数均高于0.999,加标回收率为93%～99%,检出限为0.0003～0.1275μg·mL-1,RSD值均小于2%;利用本法对5个厂家使用的碳酸锂原料药进行测定,结果表明C厂的原料药中钙、钠、镁、铁和铝元素含量均高于其余4个厂家,其中钠超出了药典规定限度。结论：与《中国药典》中碳酸锂原料药杂质测定方法进行比对,本试验所建立的方法测定结果与药典方法一致,且方法专属性强、灵敏度高、操作简单,可以用于碳酸锂原料药中6种杂质元素的测定。     

PLA/CoFe_2O_4载药微球的制备、表征及释药性能

采用 乳化-溶剂挥发法制备了聚乳酸(polylactie acid,PLA)载硫酸庆大霉素复合微球.通过正交设计实验优选PLA载药微球的最佳实验条件.在此基础上利用微乳法制备的铁酸钴(CoFe2O4)制备了PLA/CoFe_2O_4载硫酸庆大霉素复合微球.通过透射电子显微镜(TEM)、X-射线衍射(XRD)、振动样品磁强计(VSM)对铁酸钴进行微观结构表征和性能分析.采用傅立叶变换红外光谱(FT-IR),扫描电子显微镜(SEM)、生物数码显微镜对聚乳酸载药微球和PLA/CoFe_2O_4载药微球进行了微观结构的表征和分析.结果 表明两种载药微球呈规则球形,表面光滑,分布较均匀,平均粒径约为20μm.通过体外模拟释药试验考查了PLA载药微球和PLA/CoFe_2O_4载药微球的释药性能.结果 表明聚乳酸作为药物载体具有明显的药缓控释作用,PLA/CoFe_2O_4载药微球药物释放持续的时间最长.     

研究蒙脱石原料及其散剂的粒度与晶体杂质

目的:建立更为有效的激光粒度法与X-射线衍射法测定国产蒙脱石原料及其散剂的粒度与晶体杂质。方法:粒度测定:使用马尔文2000激光粒度仪,在800 mL水中以3000 r·min-1搅拌15 min,湿法测定。晶体杂质测定:采用X-射线衍射法;阴极:铜;滤过片:镍;电源:45 kV、40 mA;狭缝:0.1°;衍射角(2θ)从2°到80°扫描。结果:考察的5个企业15批蒙脱石原料中,60%均检出致癌物方英石;生产蒙脱石散的20个企业样品65%的产品检出方英石。结论:激光粒度法更为真实地反映了蒙脱石粒度的分布情况,可明显区分不同企业蒙脱石粒度的差别。X-射线衍射法可有效控制蒙脱石及其散剂中致癌物方英石的量。     

支气管哮喘,慢性肺心病患者头发中金属元素测定的临床意义

近20年有关金属元素与人类疾病的关系有较多报道,但有关支气管哮喘及慢性肺心病患者头发中金属元素含量变化的研究较少,近年我们分别测定了上述疾病患者头发中锌(Zn)、铜(Cu)、铁(Fe)、钙(Ca)、镁(Mg)及锰(Mn)的含量,探讨其含量变化与疾病的关系,兹报告如下。     

Influence of pharmaceutical excipients on stability of pramipexole dihydrochloride monohydrate in tablets

The purpose of this study was to evaluate the effect of the method of excipients addition (intra-granularly or extra-granularly) and type of excipients on the stability of pramipexole dihydrochloride monohydrate (PRM) tablets. Corn starch, pre-gelatinized starch, dibasic calcium phosphate, microcrystalline cellulose or lactose anhydrous were used as excipients. PRM tablets were prepared by a wet granulation method and stability tests were performed at 40 °C/75 % RH, 60 °C or 80 °C. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) were used to characterize the physicochemical properties of PRM. While PRM raw material was inherently stable, decreased content and increased related substances were detected for PRM tablets. By incorporating pre-gelatinized starch with the drug intra-granularly, the most stable PRM tablet formulation was achieved. The results of XRD, SEM and EDS suggested that PRM was at the surface of granules with an amorphous state. In general, as the amorphous form is more reactive than the crystalline form, compatibility between PRM and the excipient plays an important role for drug stability in the tablet. Therefore, it is essential to select proper excipients to improve stability of PRM tablets prepared using the wet granulation method.     

Determination of inorganic elements in poppy straw by scanning electron microscopy with energy dispersive spectrometry as a means of ascertaining origin

Cultivation of poppy as a source of opium alkaloids for legitimate medical purposes has a long tradition in Turkey. The main products are poppy straw and concentrate of poppy straw, obtained from dried poppy capsules. The aims of the study reported in the present article were to establish inorganic element profiles for the poppy-growing provinces of Turkey by means of x-ray analysis by scanning electron microscopy with energy dispersive spectrometry (SEM/EDS) and to explore the potential of the technique for determination of origin. Ten elements (sodium, magnesium, silicon, phosphorus, sulphur, chlorine, potassium, calcium, copper and zinc) were analysed in poppy straw samples from 67 towns in nine provinces. As regards the determination of origin, the most significant finding was the presence of copper and zinc in the poppy straw samples from 8 of the 15 towns in Afyon Province. Since those elements are not normally found in soil, it is assumed that their presence is the result of environmental (industrial) contamination. Differences in the samples from the other eight provinces were less significant, possibly a result of their geographical proximity. Nevertheless, differences in the samples were apparent. Because the findings are relative rather than absolute in terms of presence or absence of individual inorganic elements, further research is required to convert them into operationally usable results. The inorganic element profiles generated in the study have been used to form the basis for the development of a comprehensive database on poppy straw samples, which may be used in comparing samples and determining their origin.     

微量元素钙镁锌铁铜与妊娠期高血压疾病的关系

目的探讨孕妇妊娠期高血压疾病时母、脐血中微量元素钙、镁、锌、铁、铜含量与病情程度的关系以及母、脐血间有无差异。方法用日立7600型自动生化分析仪及罗氏自动生化分析仪测定正常晚期妊娠孕妇血清28例、新生儿脐血清31例及妊娠期高血压疾病患者血清及脐血清各62例的钙、镁、锌、铁、铜血清含量并进行对照研究。结果①妊娠期高血压疾病患者血清及新生儿脐血清锌、钙、镁含量显著均低于正常对照组(P<0.01)、血清铁、铜含量显著均高于正常对照组(P<0.01);且重度患者血清及新生儿脐血清锌、钙、镁含量显著均低于轻度(P<0.01)、血清铁、铜含量显著均高于轻度(P<0.01)。②从正常孕妇与妊娠期高血压疾病患者血清与脐血血清锌、铜、铁、钙、镁含量的比较中可以看出,孕妇血清锌、铁、钙、镁含量均显著低于脐血清锌、铁、钙、镁含量(P<0.05),孕妇血清铜含量显著高于脐血清铜含量(P<0.01)。结论①血清微量元素锌、钙、镁的减少,铁、铜的升高可能与妊娠期高血压疾病的发生、发展有一定的关系。②无论孕妇机体在正常状态下还是在病理状态下,都首先保证胎儿对锌、铜、铁、钙、镁的需要。     

佛山地区妊娠期妇女血液微量元素检验结果分析

目的 了解佛山地区妊娠期妇女血液中微量元素的含量,为合理的孕期保健提供科学依据.方法 选取佛山地区2013年8月至2014年7月产科门诊1573例妊娠期妇女及320例健康非妊娠妇女,均进行微量元素检测.结果 妊娠期妇女外周血的铁、钙、镁、铜以及锌的含量分别为(7.78±0.80)mmol/L、(1.67±0.11)mmol/L、(1.33±0.13)mmol/L、(91.55±15.82)μmol/L和(24.41±6.13)μmol/L,明显低于对照组(P＜0.05).妊娠期妇女的钙、铁和锌的缺乏率与对照组相比差异有统计学意义(P＜0.05).结论 佛山地区妊娠期妇女铁、钙、锌3种微量元素缺乏率较高,其中以铁缺乏最为普遍,其次为钙、锌,妊娠期妇女应合理补充微量元素,以保证孕妇母体健康和胎儿的正常发育.     

Use of back-scattered electron imaging as a tool for examining matrix structure of calcium pectinate

The internal structure of pharmaceutical solid dosage forms is commonly revealed by secondary electron imaging using standard scanning electron microscopy (SEM) technique. In this work we propose a back-scattered electron imaging (BEI) as a new tool for examining the matrix structure of calcium pectinate beads. Imaging samples with back-scattered electrons in the SEM is based on material or atomic number contrast. High atomic number elements, such as calcium, reflect more electrons and appear bright on electron micrographs. The BEI-SEM images of calcium pectinate matrix beads clearly showed net-like structure of calcium pectinate and uniform distribution of drug particles. The matrix compositions were confirmed by energy dispersive analyzer. The result demonstrates the advantageous of BEI for examining the matrix structure of calcium pectinate.     

835例儿童全血微量营养素检测分析

目的：了解深圳市盐田区儿童体内微量营养素锌、铁、铜、钙、镁和有害微量营养素铅、镉的情况。方法：选择2007年1月～2010年1月来深圳市盐田区妇幼保健院儿保门诊体检的健康儿童835例,采用北京博晖创新光电技术股份公司生产的BH5100型多通道原子吸收光谱仪和BH2100型金属炉原子吸收光谱仪,对儿童末梢全血进行锌、铁、铜、钙、镁、铅、镉7种元素含量检测,并进行统计分析。结果：深圳市盐田区学龄前儿童52.33%缺锌、43.47%缺铁、11.86%缺钙、4.43%高铅。结论：及时准确地了解儿童全血中微量营养素的含量对指导儿童平衡膳食,维持儿童正常生长发育意义重大。     

Effects of hexagonal boron nitride on dry compression mixture of Avicel DG and Starch 1500

The objective of this study was to investigate the lubrication properties of hexagonal boron nitride (HBN) on a (1:1) binary mixture of Avicel DG and Starch 1500 after using the dry granulation–slugging method and compare it with conventional lubricants, such as magnesium stearate (MGST), glyceryl behenate (COMP) and stearic acid (STAC). MGST is one of the most commonly used lubricants in the pharmaceutical industry. However, it has several adverse effects on tablet properties. In our current study, we employed various methods to eradicate the work hardening phenomenon in dry granulation, and used HBN as a new lubricant to overcome the adverse effects of other lubricants on tablet properties. HBN was found to be as effective as MGST and did not show any significant adverse effects on the crushing strength or work hardening. From the scanning electron microscope (SEM) images, it was concluded that HBN distributed better than MGST. As well as showing better distribution, HBN’s effect on disintegration was the least pronounced. Semi-quantitative weight percent distribution of B and N elements in the tablets was obtained using EDS (energy dispersive spectroscopy). Based on atomic force microscope (AFM) surface roughness images, formulations prepared with 1% HBN showed better plastic character than those prepared with MGST.     

318例孕产妇微量元素检测结果分析

目的了解目前湖北宜都地区孕产期妇女微量元素缺乏情况,为孕产妇合理补充微量元素及优生优育提供临床指导。方法采用原子吸收光谱法对孕产妇全血进行铜、锌、钙、镁、铁5种微量元素检测,并对结果进行统计分析。结果孕产期妇女铜、锌、钙、镁、铁5种微量元素缺乏率分别为1．3％、21．1％、32．4％、0．3％、22．6％。结论湖北宜都地区孕产期妇女铜、锌、钙、镁、铁5种微量元素以钙缺乏最为普遍,铁、锌次之,因此应加强孕产期妇女钙、铁、锌的合理补充．以保证母体健康和胎儿正常身心发育。