卷烟中镉成分分析标准物质的研制

目的该标准物质的研制对卷烟中镉的分析质量进行准确评价和卷烟中镉指标的安全性评价提供客观、科学的依据。方法根据国家一级标准物质技术规范（JJG 1006-94）的要求进行研制。结果该标准物质采用原子吸收光谱法和等离子发射光谱法2种不同原理分析方法进行定值。按格拉布斯法则判断每组数据，正态性D检验确认6组定值的实验数据为正态分布。标准物质总算术平均值和标准偏差分别为5．1和0．4mg/kg。结论该标准物质研制过程和结果符合国家一级标准物质的要求，申请国家一级标准物质、     

密闭高压消化ICP-MS测定茶叶等植物性样品中15种痕量稀土元素

目的：为了开展植物性样品中稀土元素含量的日常检测分析工作。方法：该文用HNO3＋H2O2在密闭高压条件下消化样品，采用标准加入法，以ICP—MS直接测定了植物样品中痕量稀土元素的含量。对消化方法、测定方式和等离子体质谱测定条件进行了优化选择，以优化后的方法分析了国家标准物质茶叶GBW07605和灌木枝叶GBW07603。结果：测定值与参考值对照，准确度为90％～110％，RSD〈5％，仪器检出限为50～70ng／L。并以该方法分析测定了国内外不同品种的茶叶的稀土元素含量。结论：该方法能够满足日常检验要求，准确可靠，快速灵敏。可以作为国标方法的一种完善和补充。     

微波消解/ICP-MS同时测定人参中15种稀土元素

目的:建立一种电感耦合等离子体质谱法测定人参中稀土元素的方法。方法:样品经HNO3+H2O2微波消解后,用ICP—MS测定89Y,139La,140Ce,141Pr,146Nd,147Sm,151Eu,157Gd,159Tb,163Dy,165Ho,166Er,169Tm,172Yb和175Lu共15种稀土元素。结果:15种稀土元素的检出限分别在0.24~2.46μg/kg之间,线性良好,相关系数≥0.9996。利用该方法分析了国家一级灌木枝叶标准物质(GBW 07604)、小麦粉标准物质(GBW 10011)和鸡肉标准物质(GBW 10018)中的稀土元素,结果与标准值一致,用该方法测定人参中的稀土元素,结果令人满意。结论:该方法质谱图简单,选择性和灵敏度好,定量准确,适用于人参中稀土元素的测定。     

水污染分析校准用硒溶液标准物质的研制

研制了国家级分析校准用硒溶液标准物质,作为硒元素的分析检测标准。依据国家标准样品工作导则要求,用重量法制备硒溶液标准物质;采用国家标准氢化物原子荧光法对样品进行均匀性和稳定性研究;并进行不确定度评估。经检测,硒标准物质均匀性良好,稳定期可达36个月以上。样品量值准确,与美国同种标准物质进行比对具有可比性。研制的硒标准物质符合国家标准物质的技术要求,已获批为国家级标准物质。可用于水中硒检测的测定标准,质量控制,分析方法研究以及分析实验室能力验证等方面。     

水质检测质量控制用钼标准样品的研制

研制国家级水质钼标准样品,作为钼分析检测的质量控制标准。依据国家标准样品工作导则要求制备钼标准样品;采用电感耦合等离子体质谱法对样品进行均匀性和稳定性研究;以7个实验室协作分析定值的统计结果确定标准值,并进行不确定度评估。结果显示,钼标准样品均匀性良好,稳定性可达24个月以上;样品量值准确,与美国同种标准物质进行比对,具有可比性。提示研制的钼标准样品符合国家标准样品的技术要求,标准编号为GSB07-3177-2014;可用于水质钼元素检测的质量控制、分析方法研究以及分析实验室能力验证等方面。     

密闭高压消化ICP-MS测定茶叶中15种痕量稀土元素

目的为了开展植物性样品中稀土元素含量的日常检测分析工作。方法该文献用HNO3＋H2O2在密闭高压条件下消化样品,采用标准加入法,以ICP—MS直接测定了植物样品中痕量稀土元素的含量。对消化方法、测定方式和等离子体质谱测定条件进行了优化选择,以优化后的方法分析了国家标准物质茶叶GBW07605和灌木枝叶GBW07603。结果测定值与参考值对照,准确度为90％～110％,RSD〈5％,仪器检出限为50ng／L-70ng／L。结论该方法能够满足日常检验要求,准确可靠,快速灵敏。     

Icp-MS在生物材料微量元素检测中的应用

用HP4500Icp-MS分析了国家标准物质中血清GBW（E）09006、冻干的尿GBW 09103、人发GBW09101全血及唾液样品中20多种元素的含量,各种样品前处理方法不同,但仪器测定条件相同,测定值与标准值符合很好,方法技术指标令人满意,并解决了含盐量高样品的分析问题。     

微波消解-氢化物发生-原子荧光光谱法测定海产品中痕量汞

目的:建立海产品中痕量汞的微波消解-氢化物发生-原子荧光光谱测定方法。方法:采用微波消解法对样品进行前处理,以硼氢化钾为还原剂,5%盐酸为载流,氩气为载气,利用原子荧光法对样品中的痕量汞进行测定。结果:汞在0.1μg/L～10.0μg/L范围具有良好的线性,相关系数大于0.9990,RSD在1.7%～8.8%之间。采用本法对紫菜成分分析标准物质(GBW10023)和黄鱼成分分析标准物质(GBW08573)进行了方法验证,所测结果均在标准参考值允许范围之内。结论:本法具有简便、灵敏、准确的优点,适合海产品中痕量汞的测定。     

ETAAS法测定小鼠脑铝血铝含量

本文对经压力消解器密闭消化后的小鼠脑及血样品,采用电热原子吸收光谱法(ETAAS),进行了铝含量的测定,以标准曲线法定量,其线性范围为0——200ppb。方法精密度c=4.9％,准确度是通过测定GBW09101人发标准物质来验证的。检出限为4.7ng~(Al)/ml。     

末梢血中铅、镉的石墨炉原子吸收光谱测定方法

[目的]建立一种简便、快速、准确的末梢血中铅、镉的测定方法。[方法]采集末梢血100μl加稀硝酸酸化稀释，在化学改进剂磷酸氢二铵、Triton X-100和氯化钯作用下，经石墨炉高温原子化和氘灯背景校正，应用标准加入法计算含量值。[结果]本法以国家有证标准物质GBW09133、GBW09139验证，结果相符，铅的相对偏差为-2．1％～1．0％。镉的相对偏差为-1．9％～1．1％。[结论]本法为一种易为受检者接受的快速准确的微量血中铅镉的测定方法。     

牛血铅成分分析标准物质的研制

目的 研制牛血铅成分分析国家一级标准物质.方法 根据<一级标准物质技术规范(JJG1006-1994)>和ISO 17511要求,按照剂量.效应关系,选择2头雄性健康牛,以醋酸铅为饲料添加物,按每天2～5 mg/ks体重剂量喂养,制作牛血铅模型.当牛血铅分别达到90～100、190～200、280～300μg/L时,采集牛血,分装于密封性良好的耐低温管中,辐射后冷冻保存.进行均匀性检验、稳定性监测及放置室温时间检验.选用核素稀释质谱法(isotopic dilution mass spectrometry,ID-MS)为研制物质铅含量赋值.通过对美国NIST SRM 955b两个浓度样品铅含量的表达验证赋值方法.结果 铅含量分别为90～100、190～200、280～300 μg/L的低、中、高浓度组研制物质均匀性单因素方差分析F值分别为0.61、1.64、0.28,P值均大于0.05,说明3组研制物质均匀.经过14个月监测,3组浓度相对标准偏差分别为0.85%、1.05%和0.49%;与14个月前比较,t值分别为0.787、1.132、0.854,P值均大于0.05,表明研制物质14个月时间数值稳定.3组牛血铅的特性量值±不确定度分别为(102.4±5.5)、(181.2±4.0)、(304.5±3.9)μg/L.通过对美国NIST SRM 955b两个浓度样品铅含量的准确重现,说明赋值方法和程序正确.置常温下4 d内测定,结果稳定.结论 该络合型牛血铅成分分析研制物质的各项指标均达到国家一级标准物质的要求.     

冻干人尿中镉标准物质的研制

目的研制冻干人尿中镉标准物质。方法采集正常人尿经处理后作为基质,通过加标、混匀、分装、冷冻干燥制备而成;经均匀性检验、稳定性考察后,由7家实验室采用2种方法进行合作定值,并进行不确定度评定。结果研制的标准物质最小取样量为0.20 ml,2个水平的均匀性检验值F分别为1.69和1.49,差异无统计学意义(P>0.05)。冻干标准物质在≤4℃下保存可稳定12个月,复溶后的标准物质溶液在4℃条件下可稳定7 d。2个水平的标准量值及不确定度分别为(5.34±0.34)μg/L和(15.47±0.72)μg/L(k=2)。结论研制的标准物质各项指标符合国家相关要求,可用于人尿中镉检测方法验证及相关样品检测。     

The influence of the closure format on the storage stability and moisture content of freeze-dried influenza antigen

Low moisture content is seen as crucial to achieving long term stability of freeze dried biologics and reference materials. Highly hygroscopic freeze-dried material are susceptible to moisture ingress over time which can lead to degradation and loss of biological potency. This study compared vials with unprocessed stoppers, vials with vacuum-oven dried stoppers and glass ampoules in order to determine the superior long term storage format in terms of moisture ingress and potency. B/Phuket influenza antigen was chosen as the model biological standard and the lyophilized antigen was stored at −20, 25 and 45 °C over a 1 year period. Ampoules had no significant moisture change across all storage temperatures as would be anticipated. Moisture content results at −20 °C showed no significant differences between ampoules, vials with vacuum-oven dried stoppers and vials with unprocessed stoppers over 12 months. Vials with vacuum-oven dried stoppers performed similarly to ampoules at −20 °C and 20 °C, but had a small increase in moisture content after 6 months at 45 °C. Vials with unprocessed stoppers preformed the worst and exhibited the largest moisture ingress after just 3 months at both 20 °C and 45 °C. Single radial immunodiffusion (SRD) potency assays showed at −20 °C and 20 °C there was no significant difference between all closure formats. At 45 °C there was a drop in potency for all closure formats, but ampoules and vials with vacuum-oven dried stoppers retained higher potency than vials with unprocessed stoppers. Thus, while ampoules are still considered to be the gold standard format for long term storage stability, using vials with vacuum-oven dried stoppers provides comparable stability and moisture integrity at −20 °C and 20 °C storage.     

Preparation and certification of lyophilized human urine for trace metals reference material in China.

The preparation of lyophilized human urine certified reference material (CRM) was established on the basis of literature in other countries and domestic conditions. The homogeneity and stability of the CRM accord with the stipulations. The certified values were determined by 14 high level laboratories in China using nine methods with different principles and have been examined by the National Institute for Occupational Safety and Health (NIOSH) using Inductively Coupled Plasma--Mass Spectrometry (ICP-MS). This CRM has been approved as first grade national reference material. It can be used in quality control of routine analysis, test of new methods, and as standard material for calibration of analytical instruments and as certified reference material for quantity transmission and analysis arbitration.     

自动顶空气相色谱法测定血液中的乙醇

目的:探讨自动顶空气相色谱法测定血液中的乙醇。方法:取一定量的血液样品,加入叔丁醇作为内标,用顶空自动进样气相色谱火焰离子化检测器进行检测,以保留时间定性,内标法、峰面积比进行定量分析。结果:乙醇浓度在0.10 mg/ml～3.00 mg/ml范围内有好的线性(r=0.9999),检出限为0.01 mg/ml,样品的加标回收率为97.8%～104.3%,RSD<2.0%。结论:所建立的方法简便、快速、准确,可用于血液中乙醇含量的检验。     

Development of a lyophilized soybean paste certified reference material for the analysis of ochratoxin A

A certified reference material (CRM) [²KRISS CRM # 108-10-018] for the analysis of ochratoxin A (OTA) in doenjang (fermented soybean paste and popular food in Korea) was produced to ensure the reliability of analytical results in testing laboratories. A home-made doenjang was chosen as a raw material after testing its OTA level. The raw material was freeze-dried, pulverized, sieved and homogenized. An isotope-dilution-liquid chromatography/tandem mass spectrometric method (ID-LC/MS/MS) which was previously developed and validated in this laboratory was used as a higher-order reference method for characterization, homogeneity studies, and short-term stability studies. The CRM had good between-bottle homogeneity with 0.56% relative standard deviation among 10 selected units. The stability of the CRM at −70 °C (the storage condition in our laboratory) and at −20 °C (the possible storage temperature at user sites) were tested for up to 8 months. No change in the OTA content was observed within the measurement uncertainty. The stability of the CRM at room temperature (for regular use and transportation) was also tested and confirmed. The certified value was (49.50 ± 1.17) μg/kg, where the expanded uncertainty was in the confidence level of 95%.     

玉米中氟成分标准物质的研制

本文根据目前国内煤烟氟污染监测工作中对质量控制的要求,研制了玉米中氟成分标准物质(两种氟浓度)。该标准物质经均匀性检查证明,样品是均匀的,经稳定性考察稳定期已达一年。采用了三种原理不同的准确、可靠方法(离子色谱法、电极法、比色法)定值。高、低浓度玉米标样的保证值和不确定度分别为33.7±2.2和1.91±0.18μg/g。玉米氟成分标准物质並可代替其它类似生物标准物质使用,本标准物质经有关部门使用反映良好。     

玉米中氟成分标准物质的研制

本文根据目前国内煤烟氟污染监测工作中对质量控制的要求,研制了玉米中氟成分标准物质(两种氟浓度)。该标准物质经均匀性检查证明,样品是均匀的,经稳定性考察稳定期已达一年。采用了三种原理不同的准确、可靠方法(离子色谱法、电极法、比色法)定值。高、低浓度玉米标样的保证值和不确定度分别为33.7±2.2和1.91±0.18μg/g。玉米氟成分标准物质并可代替其它类似生物标准物质使用,本标准物质经有关部门使用反映良好。     

冻干人尿中汞成分分析标准物质的研制

目的 研制冻干人尿中汞成分分析标准物质.方法 冻干尿由正常人尿经过滤、加标、混匀、分装、冷冻干燥、辐射灭菌制备而成,使用原子荧光测定方法 对其均匀性和稳定性进行检验,由3家实验室用准确可靠的方法 确定标准值,并对尿中汞研制物的不确定度进行分析.结果 本研制物均匀性良好,-20 ℃保存可稳定18个月,2个水平的量值及不确定度分别为(35.6±2.1)和(50.5±3.0)μg/L.结论 尿中汞成分分析标准物质各项指标符合<国家一级标准物质研制规范>的要求,可用于实验室检测的质量控制.

Abstract：

Objective To develop the certified reference material of mercury in lyophilized human urine. Methods Human urine samples from normal level mercury districts were filtered, homogenized,dispensed, lyophilized and radio-sterilized. Homogeneity test, stability inspection and certification were conducted using a atom fluorescence spectrophotometric method. The physical and chemical stability of the certified reference material were assessed for 18 months. The certified values are based on analysis made by three independent laboratories. Results The certified values are as follows: low level was (35.6±2.1)μg/L,high level was (50.5±3.0) μg/l. Conclusion The certified reference material of mercury in lyophilized human urine in this research reached the national certified reference material requirements and could be used for the quality control.     

农药致癌性的研究进展

目的研究制备适合于蔬菜基质中农药残留检测的能力验证样品, 通过能力验证评价相关实验室检测能力。方法选择卷心菜为样品基质,采用冷冻干燥、标准添加的方式制备能力验证样品,通过随机抽样测定以评估样品的均匀性,通过观察样品42天内目标化合物测试结果变化以评估样品的稳定性。结果样品均匀性及稳定性检验符合预期效果,制备的能力验证样品定值准确。结论制备的联苯菊酯、溴虫腈和氟虫腈能力验证样品,可用于蔬菜中农药残留的能力验证和方法评价,结果满意。