液相色谱-串联质谱法同时测定饲料中矮壮素和缩节胺的残留

本文采用高效液相色谱-串联质谱(HPLC-MS/MS)同时测定饲料中的矮壮素和缩节胺残留。样品先用正己烷脱除油脂,后用缓冲溶液(含0.2%甲酸-0.05mol/L乙酸铵)提取,离心上清液用乙腈沉淀净化后进行测试。结果表明:两种化合物在1.0~50.0μg/L范围内线性关系良好;定量限(S/N=10)矮壮素为0.32μg/L,缩节胺为0.45μg/L;加标回收率为91.7%~94.3%;相对标准偏差3.9%~6.1%;实测有30%的样品中含有矮壮素或缩节胺,含量范围为:矮壮素11.2μg/kg-78.4μg/kg;缩节胺9.7μg/kg-126.6μg/kg。该方法简便、快速、灵敏和准确,适合饲料中这两种农药残留的快速检测和定量分析。     

中药制剂中地西泮的LC/MS/MS分析方法研究

采用液相色谱串联质谱联用仪分析中药制剂中的地西泮。用乙腈-0.01mol/L乙酸铵水溶液(6+4)超声提取试样中的地西泮,离心分离,取上清液过滤膜后用LC/MS/MS进行检测。通过对提取方式和液相色谱分离条件的优化,建立了中药制剂中地西泮的LC/MS/MS检测方法。样品加标的回收率为87.6%~96.8%,相对标准偏差为3.1%~9.6%,多反应监测(选择离子对286.0/194.2及286.0/223.1)检出限为0.5μg/L。     

高效液相色谱-三重四级杆质谱法测定豆制品中二甲基黄、二乙基黄

建立一种同时测定豆制品中二甲基黄、二乙基黄的高效液相色谱-三重四级杆质谱(HPLC-MS/MS)方法。对提取溶剂及色谱条件进行优化,粉碎后的样品经乙腈提取,提取液以HPLC-MS/MS测定,外标法定量。二甲基黄、二乙基黄在3 min内流出并完全分离,两者在0.05~10μg/L范围内相关系数r2均大于0.999,二甲基黄在0.5~50μg/kg的加标回收率为90.0%~93.4%,RSD为0.5%~5.1%,二乙基黄在0.5~50μg/kg水平的加标回收率在84.6%~93.8%,RSD为1.1%~4.6%,检出限两者均为0.2μg/kg。该方法操作简捷、准确度和精密度高,适用于豆制品中二甲基黄、二乙基黄的检测。     

超高效液相色谱串联质谱法测定植物性食品中阿维菌素类药物残留

提出超高效液相色谱串联质谱法测定植物性食品中阿维菌素类药物(阿维菌素、伊维菌素、多拉菌素、甲氨基阿维菌素苯甲酸盐和乙酰胺基阿维菌素)残留量的方法。用乙腈提取溶剂样品中的目标物,经碱性氧化铝固相萃取小柱或炭黑氨基柱净化,超高效液相色谱分离后用串联质谱方法测定。以5类代表性植物性食品样品为基体,分别进行了4μg/kg、20μg/kg和100μg/kg3个添加水平的5种目标化合物的加标回收实验,回收率分别为80.6%～99.8%,RSD分别为0.22%～6.4%。该方法简单快速,并且方法的灵敏度、准确度和重复性均满足农药多残留分析的要求。     

含油脂食品中邻苯二甲酸酯的前处理及其GC-MS测定方法

建立了15种邻苯二甲酸酯的提取-固相萃取净化-气相色谱/质谱检测分析方法。讨论了含油脂食品中邻苯二甲酸酯的提取、净化方法,优化了色谱分离条件。研究表明,该前处理方法具有较高的净化效率,且缩短了整个检验所需时间;15种邻苯二甲酸酯的方法线性范围为50～2000μg/L,相关系数均大于0.999,加标样品在200μg/L和2000μg/L两个浓度水平下,相对标准偏差在1.1%～11.2%范围,除邻苯二甲酸二甲酯较低外,样品加标回收率均在70%～120%之间。检测限在0.07～1.2μg/L范围(S/N=3)。     

固相萃取-超高效液相色谱法测定化妆品中6种硝基酚

建立了同时测定化妆品中6种硝基酚的固相萃取-超高效液相色谱分析方法。样品采用乙腈为提取溶剂,经超声提取后再做高速离心处理;上清液以Oasis HLB固相萃取柱净化,收集甲醇洗脱液,采用色谱分析。液相色谱分析方法:选择全氟苯基色谱柱,以乙腈和乙酸铵及0.1%甲酸作为流动相,梯度洗脱,检测波长为220nm,在优化的固相萃取前处理和液相色谱分离分析条件下,净化效果满足要求。6种硝基酚类化合物在20min内实现完全基线分离,检出限为0.02~0.04mg/L,回收率为86.3%~103.6%,相对标准偏差为3.4%~7.1%。本方法准确、快速、灵敏度高,可用于化妆品的实际检验。     

土壤标准样品中有机氯农药的加速溶剂萃取/净化方法优化

通过优化土壤标准样品中有机氯农药的加速溶剂萃取/净化方法的最佳条件。结果表明:采用正己烷-二氯甲烷混合溶剂(1∶1,ν/ν)为提取剂,萃取温度100℃,压力为2 000 psi,循环1次萃取15 min,经弗罗里硅土固相萃取柱净化,气相色谱/质谱法进行检测,空白加标回收率为72%~122%,相对标准偏差介于1.0%~2.3%之间;基体加标回收率为64%~140%,相对标准偏差介于1.8%~3.2%之间;方法检出限为0.58~44.2μg/kg,定量限为1.94~147μg/kg,相比于索氏提取法,该方法简单、快捷、经济,已用于实际土壤样品中有机氯农药的检测。     

液相色谱串联质谱法同时测定动物源性食品中金刚烷胺、金刚乙胺残留量

建立了液相色谱串联质谱法测定动物源性食品中金刚烷胺、金刚乙胺残留的分析方法,以甲醇-1%三氮乙酸(50+50,v/v)作提取溶剂,用MCX固相萃取柱进行净化浓缩,内标法定量。结果表明,在ESI正离子模式下,采用多反应监测模式进行测定时,金刚烷胺和金刚乙胺的检出限为0.5μg/kg,回收率为76.7%~118.7%,相对标准偏差为1.7%~6.8%。该方法检出限低,可用于实际样品的测定。     

分散固相萃取-超高效液相色谱-串联质谱法测定动物源性食品中金刚烷胺、金刚乙胺残留量

建立了液相色谱串联质谱法测定动物源性食品中金刚烷胺、金刚乙胺残留的分析方法。通过优化提取溶剂、超声时间、提取次数确立了最佳提取条件,采用分散固相萃取净化,内标法定量。结果表明,在ESI正离子模式下,采用多反应监测模式进行测定时,金刚烷胺和金刚乙胺的检出限为0.5 μg/kg,回收率为88.4%~109.9%,相对标准偏差为2.9%~6.7%。该方法检出限低,可用于实际样品的测定。     

三重串联四级杆液质联用仪检测糖果中三聚氰胺

本文建立了高效液相色谱串联质谱检测糖果中三聚氰胺的方法。以糖果为基质,采用三氯乙酸水溶液超声提取目标分析物,提取液经过离心、净化处理后,用强阳离子交换与反相C18混合填料色谱柱分离,乙腈和l0mmol/L乙酸铵作为流动相(1:1),用串联质谱在多级反应监测模式下定量检测。LC-MS/MS定量限为0.01mg/kg,线性范围为10～500μg/L,相关系数r20.99,平均回收率为66.8%～98.7%,相对标准偏差为1.9%～7.6%(n=6)。     

Insertion of triangulated surfaces into a meccano tetrahedral discretization by means of mesh refinement and optimization procedures

In this paper, we present a new method for inserting several triangulated surfaces into an existing tetrahedral mesh generated by the meccano method. The result is a conformal mesh where each inserted surface is approximated by a set of faces of the final tetrahedral mesh. First, the tetrahedral mesh is refined around the inserted surfaces to capture their geometric features. Second, each immersed surface is approximated by a set of faces from the tetrahedral mesh. Third, following a novel approach, the nodes of the approximated surfaces are mapped to the corresponding immersed surface. Fourth, we untangle and smooth the mesh by optimizing a regularized shape distortion measure for tetrahedral elements in which we move all the nodes of the mesh, restricting the movement of the edge and surface nodes along the corresponding entity they belong to. The refining process allows approximating the immersed surface for any initial meccano tetrahedral mesh. Moreover, the proposed projection method avoids computational expensive geometric projections. Finally, the applied simultaneous untangling and smoothing process delivers a high‐quality mesh and ensures that the immersed surfaces are interpolated. Several examples are presented to assess the properties of the proposed method.     

Certification Institutions Expected to Update and Transfer Information on Present Standards

Standards are the basis for production enterprises to organize production, ex-factory inspection, trade (delivery) and technical exchanges, product certification, quality arbitration and supervision.……     

Flow calorimeter for enthalpy increment measurements on condensed gases

A flow calorimeter for enthalpy increment measurements on condensed gases is presented. A better knowledge of the properties of the liquefied natural gas is needed, and therefore a liquid loop has been designed for our flow calorimeter. The fluid loop in the calorimeter is designed in order to avoid the two-phase region, since two phases would give compositional disturbances in the measurements. The avoidance of the two-phase region is made possible by increasing the pressure of the test fluid after the measurement section, then heating the fluid at super-critical pressure past the critical point. Finally, the fluid is throttled to the low-pressure gas state at the inlet condition of the compressor that circulates the fluid. To perform the pressure increase, a new cryogenic pump has been designed. To evaluate the new equipment, measurements were taken on liquid ethane over the temperature range 146–256 K at pressure between 0.9 and 5.1 MPa.     

Refrigerators Enter a New Era of Health Preservation Frestech initiates the establishment of China's first standard for household sterilization refrigerators

On November 30, 2007, the China Association for Standardization (CAS) held a press conference at Beijing Diaoyutai State Guest House. Leaders from the China Household Electric Appliance Research Institute, the China Household Electric Appliance Association, and the China Consumers' Association attended and made speeches.……     

Optimum-Simulation von Ernteprozessen

Zusammenfassung Bei der Gestaltung von Ernteprozessen — beispielsweise des Prozesses Mähdrusch, Körnertransport und -abnahme — als transportverbundene Fließarbeitsverfahren mit mindestens zwei verschiedenen Arbeitsmitteln gibt es einen großen Optimierungsspielraum. Solche Prozesse sind mehrstufige Bedienungsprozesse mit gemischter Anordnung der Bedienungseinrichtungen. Außerdem besitzen sie stark ausgeprägte räumliche Aspekte. Es wird vor allem gezeigt, welche Merkmale solcher Prozesse in Simulationsmodellen abgebildet sein müssen, welche Zielgrößen in Abhängigkeit von welchen Einflußgrößen unter Berücksichtigung welcher Prozeßbedingungen ermittelt werden sollten und wie der Bewertungsprozeß zur Ermittlung der gewünschten Informationen gestaltet werden muß.     

A study of centrifugal cast high boron high speed steel

In the present study a high‐boron high speed steel (HSS) roll material was designed. Many expensive alloy elements have been substituted by cheap boron alloy, and high‐boron high speed steel roll has been manufactured by centrifugal casting method. The microstructures, mechanical properties and wear resistance of centrifugal casting high‐boron high speed steel roll have been investigated by optical microscopy (OM), scanning electron microscopy (SEM), and X‐ray diffraction (XRD) analysis, hardness test, impact test and wear test. The results indicated that the solidification microstructures of high‐boron high speed steel roll consisted of M₂(B,C), (W,Mo)₂(B,C), M₃(B,C), M₂₃(B,C)₆ type borocarbides and martensite, a small amount of retained austenite. Borocarbides were continuously distributed over the grain boundary. After quenching from 1050 °C, local broken network appeared in partial borocarbides, and fine secondary borocarbide precipitated from the matrix. After tempering from 525 °C, the amount of precipitated borocarbide increased significantly. After heat treatment, the hardness of high‐boron high speed steel roll excelled 60 HRC, and its impact toughness excelled 8.0 J/cm². The single groove steel rolling amount of high‐boron high speed steel rolls increases by 500% than that of bainite cast iron roll, when the rolls are used in K₁ mill housing of bar mill.     

Thixotropy of Systems with Shear Thinning and Plastic Flow Behavior

The definition of the thixotropy is a decrease in viscosity with time in shear and a subsequent recovery of viscosity after the shear deformation is removed.We ...     

Brainstorming for ISO Strategy 2016-2020

正Responding to ISO’s appeal for survey for the to-be-developed ISO Strategy Plan for 2016-2020,SAC hosted a special workshop over the needs and comments of various fi elds on June 8 in Beijing.The workshop was attended by ISO President-elect and Ansteel General Manager Zhang Xiaogang,SAC Vice-Administrator Yu Xinli,and 30 experts from     

CNAS Passes APLAC's PTP Review

正The review group of Asia Pacific Laboratory Accreditation Cooperation(APLAC)carried out a 4-day peer review of the proficiency testing provider(PTP)for China National Accreditation Service for Conformity Assessment(CNAS)from July 28 to 31,2014.CNAS passed the PTP review with excellent performance.Two senior peer reviewers of APLAC made a comprehensive,rigorous and detailed review of CNAS’s PTP accreditation activities,and made the on-spot inspection of the review groups in Shanghai and Shenzhen respectively.