用经验模型评估环境样品测量不确定度

利用水样、土壤和沉积物标准样品定值数据,建立了评估环境样品测量结果不确定度的经验模型。讨论了判断模型质量的指标。用建立的经验模型估算了实际标样和能力验证数据不确定度,并与实测结果进行了比较。探讨了利用本模型计算的相对标准偏差允许限用于实验室内部质量管理与控制的可行性。经验模型能帮助客户判断送检样品检测结果在临界值时能否满足相关要求。     

气相色谱法测定广藿香油中百秋李醇含量

建立了气相色谱仪测定广藿香油中百秋李醇含量的方法。用毛细管色谱柱DB-5MS（30m×O．32mm．0．25μm）,正十八烷为内标,氢火焰离子化检测器进行检测,内标法定量。百秋李醇含量在0．2-2．0mg／mL范围内,百秋李醇峰面积和内标物峰面积之比与百秋李醇质量浓度呈良好的线性关系,相关系数r=0．9997。方法的检出限为1μg／mL,加标回收率为90．0％～100．6％,测定结果的相对标准偏差为1．22％（n=6）。研究表明,本法简便、快速、测定结果准确可靠,精密度优于外标法。     

Simple method for the determination of rosiglitazone in human plasma using a commercially available internal standard

To the best of our knowledge, bioanalytical methods to determine rosiglitazone in human plasma reported in literature use internal standards that are not commercially available. Our purpose was to develop a simple method for the determination of rosiglitazone in plasma employing a commercially available internal standard (IS). After the addition of celecoxib (IS), plasma (0.25 mL) samples were extracted into ethyl acetate. The residue after evaporation of the organic layer was dissolved in 750 microL of mobile phase and 50 microL was injected on to HPLC. The separation was achieved using a Hichrom KR 100, 250 x 4.6 mm C(18) with a mobile phase composition potassium dihydrogen phosphate buffer (0.01 m, pH 6.5):acetonitrile:methanol (40:50:10, v/v/v). The flow-rate of the mobile phase was set at 1 mL/min. The column eluate was monitored by fluorescence detector set at an excitation wavelength of 247 nm and emission wavelength of 367 nm. Linear relationships (r(2) > 0.99) were observed between the peak area ratio rosiglitazone to IS vs rosiglitazone concentrations across the concentration range 5-1000 ng/mL. The intra-run precision (%RSD) and accuracy (%Dev) in the measurement of rosiglitazone were <+/-10.69 and <-12.35%, respectively across the QC levels (50-1000 ng/mL). The extraction efficiency was >80% for both rosiglitazone and IS from human plasma. The lower limit of quantitation of the assay was 5 ng/mL. In summary, the methodology for rosiglitazone measurement in plasma was simple, sensitive and employed a commercially available IS.     

中学生营养平衡米膳食最佳模式评价

根据中国营养学会推荐的热量标准,研制了中学生营养平衡米膳食最佳模式。按该模式,中学生每日应摄入的膳食品种及其数量如下:主食:营养平衡米,初中男生510~597g,女生468~510g;高中男生618~683g,女生532~575g;副食相同:青菜或水果500g或600g,鱼或肉100g或50g,蛋类40g,大豆制品30g,花生油12.5g,盐6g。调查结果表明,蛋白质、脂肪、碳水化合物,热量摄入量全部达标准要求。Q(蛋白质)∶Q(脂肪)∶Q(碳水化合物):高中男女生为16∶20∶64,初中男、女生分别为17∶20∶63。提示中学生营养平衡米膳食最佳模式使中学生达到营养平衡,建议推广食用。     

ICP-AES内标法测定分子筛的组成

首次通过ICP-AES仪研究了分子筛化学组成全分析的方法，采用HNO3-HF混合酸密闭溶样，用H3BO3配合F^-，分别采用内标法和基体消除法消除基体效应．将研究结果与经典方法比较表明：采用本文研究的分析方法，结果准确可靠，符合分析要求，尤其对杂原子分子筛以及金属氧化物修饰的分子筛的组成分析具有应用价值．     

Thermochemistry of the complexes of chromium nitrate with l-a-amino acids

The solid complexes of Cr(NO₃)₃ with L-α-amino acids (AA=Val, Leu, Thr, Arg, Phe and Try) have been prepared in 95% alcoholic, the compositions of which were identified as the general formula Cr(AA)₂(NO₃)₃·2H₂O by elemental and chemical analyses. The bonding characteristics of the title complexes were characterized by IR, indicating that nitrogen and oxygen atoms in the ligands coordinated to Cr³⁺ in a bidentate fashion. With the aid of TG-DTG and IR techniques, the complexes were subjected to thermal decomposition in an atmosphere of oxygen, presuming that the decompositions of the complexes consist of two steps and the complexes were decomposed into chromium hemitrioxide after undergoing dehydration and skeleton splitting of the complexes. The constant volume energies of combustion of the complexes were determined by a RBC-P type rotating-bomb calorimeter. According to Hess's law, the standard enthalpies of formation of the complexes were calculated as (-1831.40±4.40), (-2542.03±6.13), (-1723.81±3.99), (-2224.31±3.02), (-2911.61±6.53) and (-659.32±7.42) kJ mol^-1, respectively. This revised version was published online in August 2006 with corrections to the Cover Date.     

Summary of ISO/TC 201 standard: XXI. ISO 21270:2004—Surface chemical analysis—X‐ray photoelectron and Auger electron spectrometers—Linearity of intensity scale

This International Standard specifies two methods for determining the maximum count rate for an acceptable limit of divergence from linearity of the intensity scale of Auger and x‐ray photoelectron spectrometers. It also includes methods to correct for intensity non‐linearities so that a higher maximum count rate can be employed for those spectrometers for which the relevant correction equations have been shown to be valid. Copyright © 2004 John Wiley & Sons, Ltd.     

量热法研究氯化铒与甘氨酸配合物的标准生成焓

量热法测定;量热法研究氯化铒与甘氨酸配合物的标准生成焓     

水合六硼酸钡的合成与热化学研究

硼原子的硼酸盐种类繁多,结构复杂多样,其中,有一些硼酸盐具有特殊的性能,如:2ZnO·3B_2O_3·3.5H_2O、2CaO·3B_2O_3·5H_2O可用作阻燃材料~([1]),β-BaB_2O_4(β-BBO)~([2])、Ba_2Be_2B_2O_7~([3])、BaAl_2 B_2O7_~([4])等因其具有良好的光学性质,被广泛用作非线性光学材料.因此,进行硼酸盐的合成及性质研究有着重要的意义.     

An overview of analytical methodologies for the determination of antibiotics in environmental waters

The widespread occurrence of antibiotics as contaminants in the aquatic environment has increased attention in the last years. The concern over the release of antibiotics into the environment is related primarily to the potential for the development of antimicrobial resistance among microorganisms. This article presents an overview of analytical methodologies for the determination of quinolone (Qs) and fluoroquinolone (FQs), macrolide (MLs), tetracycline (TCs), sulfonamide (SAs) antibiotics and trimethoprim (TMP) in different environmental waters. The analysis of these antibiotics has usually been carried out by high-performance liquid chromatography (HPLC) coupled to mass spectrometry (MS) or tandem mass spectrometry (MS/MS) and to a lesser extent by ultraviolet (UV) or fluorescence detection (FD). A very important step before LC analysis is sample preparation and extraction leading to elimination of interferences and prevention of matrix effect and preconcentration of target analytes.