药品和膳食补充剂中金属含量的分析——NexION 300 ICP-MS在执行USP 232法案中的应用

美国药典(USP)提议的通用章节USP 232将替代原来的USP 231.在食品和膳食补充剂中使用的有效药物原料不可避免地包含许多元素,因此现代检测实验室已开始使用各种手段应对不断增加的食品和膳食补充剂产品中元素的检测需要.电感耦合等离子体质谱仪(ICP-MS)能够分析元素周期表中绝大多数的元素,而且检测浓度范围为μg/g～mg/g,这样的检测浓度范围表明在一次分析中可以对痕量污染物和重要的营养元素同时进行测定,因此是满足以上需求的理想选择.     

微波消解-电感耦合等离子体质谱法测定生物样品中微量硒的方法研究

生物样品中微量元素硒的分析检测,经典方法是湿法消解-氢化物发生原子荧光光谱法(HGAFS)。湿法消解处理生物样品需使用大量试剂,并且消解时间长,样品背景值高;HG-AFS的分辨率较低,已经不能满足微量硒的分析需求。解决生物样品的消解过程缓慢、试剂用量大的问题是提高样品中微量元素硒的检出限和分辨率的前提。本文采用湿法消解和微波消解两种消解体系处理样品,对两种方法制备的溶液分别采用HG-AFS和电感耦合等离子体质谱法(ICP-MS)进行测定,通过对比试验确定了微波消解ICP-MS方法可以实现生物样品中微量硒的准确测定。对比试验表明:采用高压密闭微波消解前处理样品技术可以大大缩短消解时间,减少试剂用量,降低了样品背景值;利用ICP-MS直接进行测定,方法检出限为0.01μg/g,精密度(RSD,n=12)小于4%,低于HG-AFS的检出限(0.03μg/g)和精密度(10%)。微波消解ICP-MS方法操作简单快捷,降低了方法检出限,提高了样品分析的准确度和精密度。     

微波消解电感耦合等离子体质谱法测定地球化学样品中钒铬镍锗砷

地质样品中多种元素的分析,通常采用高压密封消解电感耦合等离子体质谱法(ICP-MS),而应用于测定地球化学样品中的V、Cr、Ni、Ge、As等元素,影响分析准确度的主要原因有:样品前处理方面,高压密封罐会释放Cr和Ni污染样品,同时Ge和As属于易挥发元素容易造成损失;质谱测定方面,多原子分子离子会产生干扰。本文针对两方面的干扰因素,对比了微波消解硝酸提取、微波消解王水提取、高压密封硝酸复溶、高压密封王水复溶四种前处理方法中待测元素的溶出效果以及污染或损失情况。结果表明,采用微波消解替代高压密封罐消解可消除引入的Cr、Ni污染,避免了Ge、As挥发损失,同时微波消解的时间短。而采用硝酸提取,由于避免了氯的引入,分析效果优于王水提取。且使用八极杆ICP-MS氦气碰撞模式消除了样品基体中的氯多原子分子离子干扰(如37Cl14N对51V干扰,35Cl16OH对52Cr干扰,35Cl37Cl对72Ge干扰以及40Ar35Cl对75As干扰等)。应用微波消解硝酸提取、ICP-MS测定岩石、水系沉积物和土壤国家标准物质,V、Cr、Ni、Ge、As的检出限分别为1.09、0.19、0.55、0.02、0.50μg/g,精密度(RSD)4%,而采用高压密封消解、ICPMS测定V、Cr、Ni的检出限为3.48、13.09、21.67μg/g(Ge和As由于挥发无法用此法检测)。运用微波消解硝酸提取-ICP-MS氦气碰撞模式测定地球化学样品中V、Cr、Ni、Ge、As,简化了分析流程,样品消解时间仅2 h,相比于高压密封方法(消解时间48 h)具有消解快速、多元素同时测定、检出限低的特点。     

ICP-MS和ICP-AES测定地球化学勘查样品及稀土矿石中铌钽方法体系的建立

针对目前铌钽分析中出现的样品溶解不完全、元素易水解及现有分析技术流程复杂的情况,本文对常用的混合酸恒温电热板溶解和过氧化钠碱熔两种样品前处理方式进行优化,运用电感耦合等离子体质谱法(ICP-MS)、电感耦合等离子体发射光谱法(ICP-AES)两种技术手段,建立了测定地球化学勘查样品及稀土矿石中不同含量水平的铌、钽两套分析方法。对于铌、钽含量较低且易于分解的样品,采用硝酸-氢氟酸-硫酸混合酸恒温电热板消解ICP-MS方法测定;对于铌、钽含量高且难溶的样品,采用过氧化钠高温熔融ICP-AES方法测定。ICP-MS用于分析低含量样品更具优势,而高含量样品更适合运用ICP-AES。通过分析土壤、水系沉积物、岩石、稀有稀土矿石系列国家标准物质,结果表明混合酸处理ICP-MS分析方法的线性范围为0~200ng/mL;检出限为铌0.01μg/g,钽0.05μg/g;相对误差小于10%,精密度(RSD)小于6%;碱熔处理ICP-AES分析方法的线性范围为0~30μg/mL,检出限为铌0.2μg/g,钽2.5μg/g,相对误差小于10%,精密度(RSD)小于7%。这两套分析方法可以满足基体复杂、铌钽含量变化范围大、试样批量大的检测要求。     

风冷回流消解-电感耦合等离子体质谱法同时测定植物样品中46个元素

采用HNO3-H2O2体系对植物样品进行风冷回流消解,电感耦合等离子体质谱法(ICP-MS)同时测定植物样品中46个元素的含量。将称有样品的磨口锥形瓶加装风冷管后直接放在普通平板铝块电热板上,一次可对45个锥形瓶回流装置同时进行加热,不需要严格地规定消解时间,保证回流加热微沸消解至消解完全即可。植物标准物质(GBW 10012、GBW 10014和GBW 10019)的分析结果与标准值相一致,方法精密度(RSD,n=6)为0.44%～5.59%。与干法灰化消解和微波消解等样品处理方法相比较,操作简单快捷,试剂用量少,空白值较低,溶液盐度较小,有利于植物样品中多元素ICP-MS同时测定。采用调试液调节ICP-MS仪器测定的最佳化,确定了ICP-MS测定的最佳条件,同时探讨了元素之间的干扰关系,采用数学校正法有效地消除了测定的干扰。     

电感耦合等离子体质谱法精确测定地质样品中的微量元素镓

应用电感耦合等离子体质谱法(ICP-MS)对地质样品中微量元素镓进行测试分析时,存在两方面问题:一是不同消解方法各有不足,密闭式消解不能批量处理样品,而敞开式消解过程繁杂;二是质谱测试时需要选择⁶⁹Ga还是⁷¹Ga,确定扣除哪些干扰和相应的扣除系数,这些因素使地质样品中镓元素的测试精度不高。本文基于一般地质样品中有机质含量低的特点,针对ICP-MS分析方法提出:①使用氢氟酸、盐酸、硝酸、高氯酸四种酸混合消解样品,采用半密闭式酸分解法,通过调整加热温度、用酸量、用酸比等加快反应进程,少量的有机质在强酸加热消解时能够反应完全,而不必要进行灰化处理;②采用丰度为39.9%的⁷¹Ga进行测试,使用经验系数0.005,利用⁵⁵Mn¹⁸O对⁷¹Ga位置扣除⁵⁵Mn¹⁶O的干扰。方法精密度在3%以内,方法检出限为0.06 μg/g。本方法简化了样品消解过程,并可批量处理样品,降低了分析成本,在准确测定镓元素的同时还能理想地测定其他微量元素和稀土元素。     

微波消解-高分辨电感耦合等离子体质谱法测定土壤中8种金属元素

微波消解结合电感耦合等离子体质谱(ICP-MS)是土壤样品中金属元素测定的常用方法,其前处理可以采用不同的消解体系,但是消解体系对分析结果的准确性影响较大。此外,应用ICP-MS测定某些元素时干扰的存在会影响结果的准确性。基于上述问题,本文优选三个酸体系微波消解溶样,采用高分辨电感耦合等离子体质谱(HR-ICP-MS)测定土壤样品中8种金属元素(Cr、Co、Ni、Cu、Zn、Pb、Cd和U)的含量,对比研究了由不同用量硝酸、盐酸、氢氟酸混合组成的三个酸消解体系对国家土壤标准物质的消解效果,确定了最优前处理方法。结果表明：经国家土壤标准物质验证,采用HR-ICP-MS检测,在不需要干扰校正的情况下,酸体系Ⅰ(6mL硝酸+3mL盐酸+3mL氢氟酸)和酸体系Ⅱ(2mL硝酸+6mL盐酸+1mL氢氟酸)的测定值与标准值相吻合,方法检出限为0.001～0.715μg/g,精密度(RSD,n=6)小于7.0%。从消解情况、准确度和精密度比较,酸体系Ⅰ稍优于酸体系Ⅱ;从酸用量比较,酸体系Ⅱ酸用量最少。两种酸体系的样品处理方法均具有较高的适用性和可靠性,都可用于土壤样品中8种金属元素含量的直接测定。     

Elan DRC-e 等离子体质谱仪在食品分析中的应用

了解食品中营养元素和有害元素的组成十分重要,食品分析一般要求测定其中的高含量(mg/L)组分,也需要测定其中的低含量(μg/L)组分。传统的食品样品分析需要采用多种仪器方法,如用火焰原子吸收光谱法(FAAS)测定食品中的高含量组分,而使用石墨炉原子吸收光谱法(GFAA)测定其中的痕量组分。随着电感耦合等离子体质谱(ICP-MS)技术的不断发展,以上食品样品分析的挑战可在带有动态反应池(DRC)技术的ICP-MS上实现。目前已报道了多篇Elan DRC型ICP-MS应用于食品分析的文献[1-5]。Elan DRC型ICP-MS多项独特的设计使其非常适合于食品分析。某些高含量元素会使检测器达到饱和     

电感耦合等离子体质谱法测定地下水中44个元素

采用电感耦合等离子体质谱法(ICP-MS)同时测定地下水中44个元素。结果表明,ICP-MS可同时测定地下水中44个元素,方法检出限为0.002～0.981μg/L,大多数元素的精密度(RSD,n=10)均小于10%,加标回收率在90.0%～110.0%,符合中国地质调查局地质调查技术标准对无机组分测试质量控制的要求。方法应用于直接测定元素浓度范围在ng/L～mg/L级的实际地下水样品,快速、简便,结果准确。     

使用NexION 300 ICP-MS按照加利福尼亚州65号法案测定钙制酸剂和膳食补充剂中的铅

按照美国加利福尼亚州65号法案中对钙制酸剂和膳食补充剂中Pb的控制要求,分析方法对这类固体物质中铅的检出限要求低于0.05g/g。电感耦合等离子体质谱仪(ICP-MS)的分析能力使其成为常规检测中低含量Pb测定的最佳仪器。但是,如果不采用特定的预防措施消除潜     

Unity of the national and the international in the socio-cultural development of the peoples of the USSR

International unity is becoming ever stronger in this country owing to an increasing similarity in the development of the cultural environment. This comprises the provision of all the country's republics with a sufficient number of schools, theatres, and other institutions and cultural information media in accordance with the needs of the population. An important part is played by the rise in ‘the general educational level, as well as the level of professional qualifications and skills. Among all the Soviet nations and nationalities, this rise being more rapid among formerly backward peoples. Prominent among the factors of internationalization is the progressive development of the nationalities’ cultural resources, while professional culture is being increasingly brought within the reach of the masses.The implementation of the nationalities policy promotes the all-round development of all Soviet nations and nationalities, their drawing together, the upsurge of the individual capabilities of every Soviet citizen.     

Report of the restudy of the defined global stratotype of the base of the Silurian System

The Global Stratotype Section and Point （GSSP） for the base of the Silurian System was defined in 1985. Since that time, a number of researchers have suggested that this section has serious deficiencies for use as a GSSP. As a result, in 2000, the Subcommission on Silurian Stratigraphy （SSS） proposed undertaking a formal restu@ of this GSSP, which was subsequently approved by the International Commission of Stratigraphy （ICS）. The result of this restudy was the formal proposal that the current GSSP, at 1.6 m above the base of the Birkhill Shale, at Dob＇s Linn, Scotland, should be maintained as the same locality and stratigraphic level, but the bios- tratigraphical definition of the boundary should be revised. The previously defined, basal Silurian grapto- lite zone, the Parakidograptus acuminatus Zone, should be subdivided into a lower Akidograptus ascensus Zone and a higher E acuminatus Zone. The base of the A. ascensus Zone, marked by the first appearance of A. ascensus, should be regarded as the biostratigraphic mark for the base of the Silurian. This proposal has now been formally approved by the SSS and ICS, and ratified by International Union of Geological Sciences. This is the first GSSP to undergo formal restudy and redefini- tion, and the proposal also included a recommended procedure for restudy of GSSPs.     

Deviation of the major axis of the inertia ellipsoid of the Moon from the direction toward the Earth

It is known from observations that the center of mass of the Moon does not coincide with the geometric center of its figure, and the line connecting these two centers is not aligned with the direction toward the center of the Earth, instead deviating toward the Southeast. This stationary deviation of the axis of the inertia ellipsoid of the Moon to the South of the direction toward the Earth is analyzed. A system of five linear differential equations describing the physical libration of the Moon in latitude is considered, and these equations are derived using a new vector method taking into account perturbations from the Earth and partly from the Sun. The characteristic equation of this system is obtained, and all five oscillation frequencies are found. Special attention is paid to the fifth (zero) frequency, for which the solution of the latitude libration equations are stationary and represents a previously unknown additional motion of the rotational axis of theMoon in a cone with a small opening angle. In contrast to the astronomical precession of the Earth, the rotation of the angular-velocity vector is in the positive direction (counter-clockwise), with the period T ₃ = 27.32 days. On this basis, this phenomenon has been named “quasi-precession.” This quasi-precession leads to a stationary inclination of the major axis of the inertia ellipsoid of theMoon to the South (for an observer on Earth), making it possible to explain one component of the observed deviation of the center of mass of the Moon from the direction toward the Earth. The opening angle of the quasiprecession cone is approximately 0.834″.     

The Tendencies of the Development of the Mineral-Resources Sector at the Turn of the Century

Important tendencies in development of the world mineral-resources sector at the beginning of the 21st century were an increase in production and consumption of mineral materials differentiated by types of metals and nonmetallic mineral raw materials, by countries and regions, as well as the concentration of the production of mineral raw materials in a small number of countries, and a reduction in industrial reserves of minerals in the world economy, even at the current stage of their extraction. These tendencies should be taken into account in working out a strategy for development of the Russian mineral raw-material base.     

Causes of the famine among the rural population of the Sahelian zone of the Sudan

Taking the example of W Sudan, an analysis of the climatic incidents leading to the two recent famine disasters is made. On this natural background, the human side is investigated. Focus is directed towards the fragile economic structure of the famine-prone population groups. An early-warning system for famine in the Sahelian Zone is proposed taking grain production and storage, livestock development and the relationship between the prices of livestock and grain as major indicators.     

东濮凹陷北部沙河街组三段中亚段沉积环境分析

东濮凹陷北部沙三中亚段广泛发育盐岩和烃源岩,这两个看似不能共存的物质却在这里互层共生。该时期研究区沉积特征为多盐韵律与多层烃源岩互层共生、连续沉积,单个盐韵律厚度从几米到十几米,烃源岩有机质丰度高、类型好。平面上,两者在湖盆沉积沉降中心共生;垂向上,高有机质丰度、好干酪根类型与高盐度地层具有较好的对应关系。因而成为恢复古气候和古环境的重要研究对象。通过岩石学、古生物学以及Sr/Ba、B/Ga、(V+Ni+Mn)、Fe/Mn、Sr/Cu、Mg/Ca、V/(V+Ni)、稀土元素含量和氯同位素等方法对凹陷北部沙三中亚段的沉积环境进行研究。结果表明,凹陷北部沙三中亚段为深水沉积的还原环境,古盐度较高,达到半咸水-咸水沉积;微量元素和孢粉化石特征表明研究区沙三中亚段为温暖潮湿的环境。     

On the consistency of proposed models for the Pyrenees with the structure of the eastern parts of the belt

The structure of the eastern Pyrenees consists mainly of south-directed thrusts involving basement and cover rocks. An antiformal stack developed by the piling up of basement thrust sheets which outcrop in the Axial zone. These structures account for a thin-skinned thrust model rather than a vertical fault model in which the Axial zone would be essentially autochthonous, and the North-Pyrenean fault the axial plane of a fan thrust system. New data from the Eastern Pyrenees and the thin-skinned model suggest that(1) the structure east of the Pedraforca nappe is similar to that of the Central Pyrenees; (2) the cover rocks of the South-Pyrenean units and of the Axial zone-after restoration—built up a northwards-thickening prism consistent with the existence of a unique Pyrenean sedimentary basin during Mesozoic time; (3) the Axial zone is only a complex antiformal stack developed as a part of South-Pyrenean system related to the Paleogene thrusting-tectonics. The Axial zone palaeogeographic area had no special meaning during Mesozoic time.     

The Importance of the Precipitation and the Susceptibility of the Slopes for the Triggering of Landslides Along the Roads

In order to characterise the influence of the heavyrains on the observed landslides during the 1996–1997hydrological cycle, rainfall records for the last 100years are analysed from 104 stations in easternAndalusia. Regarding the amounts of rain recordedbetween October 1996 and March 1997 in the 104stations studied, 31 presented new all-time records;15 presented values that were 80–100% of thepre-1995 record; 49 stations, 80–50%; and 9stations, < 50%. A map has been devised of thesusceptibility of the materials through which thesouth-eastern Andalusian road network crosses,together with an inventory of the damage caused byinstability phenomena on banks and cuttings of theroad network during the winter of 1996–1997. Therelationships between the rainfall during the studyperiod, the damage caused to the road network and thesusceptibility of the materials affected are analysed.The results indicate that there is a clearcorrespondence between the rainfall recorded and thesusceptibility of the materials with the inventorieddamage. It is concluded that the widespread seriousdamage caused in early 1997 to the roads andsurrounding areas in the Alpujarra region and thecoast of the Province of Granada was mainly caused bythe extraordinarily heavy rains. However, considerablyless damage was observed where the susceptibility ofthe terrain is low, thus highlighting the extremeusefulness of terrain-susceptibility maps for riskprevention and territorial planning.