非完全消化-火焰原子光谱法测定奶粉中钙镁铁锌

用非完全消化法处理奶粉样品，建立了用火焰原子光谱法测定奶粉中钙、镁、铁、锌的快速分析方法。在低温下用浓硝酸消化奶粉至溶液透明，加乳化剂OP溶解消化过程中所产生的油脂，可获得一均匀、透明的样品溶液。以发射法测定钙，用吸收法测定镁、铁和锌。以Sr^2 作为测定钙、镁的释放剂。对样品消解每件及干扰进行了考察。测定结果的相对标准偏差小于2．4％，加标回收率在98．8％～102．0％之间。方法简便、准确。     

1152例婴儿血中6种元素检测结果的分析

为探讨婴儿体内铜、锌、钙、镁、铁和铅微量元素的含量及其与年龄、性别的关系,测定了1 152例湖南长沙地区1岁内婴儿指末梢全血中6种元素铜、锌、钙、镁、铁和铅的含量,对其结果进行了统计分析。结果表明,所测婴儿元素铁、锌缺乏最显著,其次是钙缺乏;铜、镁无明显失衡;血铅超标的水平较低;不同性别之间6种元素含量的差异无统计学意义。提示在长沙地区的孕婴保健中,应加强锌、钙与铁的合理补充。     

火焰原子吸收光谱法直接测定血清中钙铁锌

随着社会发展进步,人们越来越重视生活质量,自身的健康显得尤为重要.人体缺乏钙、铁、锌等元素,易发生骨折、贫血、发育迟缓等症状.某些疾病也可引起钙、铁、锌等元素增高[1].测定全血钙、铁、锌等元素也有报道[2],但是该分析方法在预处理过程中,需要混合酸的消化,易损失产生误差.本试验用火焰原子吸收光谱法直接测定血清中钙、铁、锌的含量,省略了消化过程.测定钙、铁时,加入基体改进剂,提高了检测钙、铁的灵敏度.此方法操作简便、快速、试剂用量少、准确度高、共存元素干扰少,对质控血清进行了钙、铁、锌的测定,结果满意.     

淮安市1684名中小学生血清钙、铁、锌含量分析

为了解淮安地区中小学生血清中钙、铁、锌含量情况,应用改进的火焰原子吸收光谱法对1684名对象的血清中相关元素的含量进行了测定。结果表明,该地区3种元素总体水平在正常范围内,钙、铁、锌血清含量分别为（102．69±26．30）mg／L、（1．01±0．61）mg／L、（0．86±0．45）mg／L;性别、城乡差别无统计学意义（P〉0．05）;而年级的差别有统计学意义（P值均〈0．0001）,初中组各元素水平明显高于小学组。     

小儿锌、铜、铁、钙缺乏症的调查及健康指导

为了解本地区小儿锌，铜，铁，钙缺乏的情况，以便更好地进行小儿营养膳食指导，对1994－2001年在我院儿科门诊就诊4891例小儿发中锌，铜,铁，钙含量进行了测定。结果表明，锌，钙，铁，铜缺乏率 ：38．5％，26．8％，16．7％，0．2％。锌缺乏率有随年龄增长而增高的趋势，而钙缺乏率则有下降趋势。可见锌，铁，钙营养不足仍是本地区小儿最主要的健康问题，应根据不同年龄进行有针对性健康教育及营养指导。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中铜、锌、钙、镁、铁

样品经硝酸-高氯酸消化溶解,高氯酸冒烟,盐酸溶解盐类后,在盐酸(5%)介质中,在选定的测定条件下,用电感耦合等离子体原子发射光谱(ICP-AES)法测定人发中微量元素铜、锌、铁、镁、钙。选择Cu 327.3、Zn 206.2、Fe 238.2、Mg 279.5、Ca 315.8nm分别作为铜、锌、铁、镁、钙的分析线与混合标准溶液同时测定;方法加标回收率为98.6%～101%,铜、锌、铁、镁、钙的精密度(RSD,n=8)为0.37%～2%,准确度(RE)为-3.4%～1.15%,检出限分别为0.002 3、0.001 6、0.004 6、0.003 0、0.001 4μg/mL。方法克服了分光光度法和原子吸收光谱法操作繁琐、周期长、成本高、灵敏度低等缺点。用于测定人发样品中的铜、锌、铁、镁、钙元素,测定结果与原子吸收光谱法测定值基本一致。经GBWO7061标准物质和自制标样分析验证,测定值与标准值吻合,结果准确可靠。     

妊娠期糖尿病妇女血清中元素含量的变化

糖尿病与体内微量元素的不平衡密切相关。妇女在妊娠期中容易发生糖耐量异常和妊娠期糖尿病,因此研究这些孕妇血清中元素含量的变化,对弄清妊娠期糖尿病的机理和进行防治有重要意义。本工作测定了糖耐量异常和妊娠期糖尿病孕妇血清中硒、铜、锶、镁、锌、钙、磷、铁和铝等九种元素持含量,研究了其与正常孕妇的差异,并观察了元素含量与孕期的相关性。结果表明,糖耐量异常和妊娠期糖尿病孕妇血清中硒的含量与正常孕妇相比明显降低。妊娠期糖尿病孕妇血清中铜比正常孕妇显著升高,而锌有降低趋势,其它元素则未明显变化。此外,观察到正常孕妇和血清异常孕妇血清中硒和钙的含量都与孕期呈明显的负相关性。     

非完全消化-火焰原子吸收光谱法测定水果中铜铁锌

用非完全消化法处理杏、油桃和草莓样品,即在低温下用浓硝酸-高氯酸(3+1)混合酸消解样品,再加入乳化剂TX-10溶解消化过程中所产生的油脂,将所得橙红色的均匀透明溶液用火焰原子吸收光谱法测定其中铜、铁和锌元素的含量.对样品处理条件、混合酸中杂质及共存TX-10的干扰进行了试验.铜、铁和锌的检出限(3s/k)分别为0.019,0.145,0.009 mg·L-1.用此法测定水果实样中铜、铁和锌的含量,所得结果与灰化法测定结果相一致.     

高钙镁铅锌矿中锌的交流示波极谱滴定

本文阐述了用交流示波极谱滴定法测定高钙镁铅锌矿中的锌。在NH_4Cl—NH_3H_2O(pH=10)支持电解质中采用微银汞膜电极进行实验。分别用NH_4F和铜试剂掩蔽钙、镁、铜、铅、镉及其它竽金属元素。铁和铝不干扰测定。用EDTA滴定锌获得令人满意的结果,对两种矿样分析,准标偏差为0.05%和0.07%。该法快速准确,适用于测定高钙镁的铅锌矿中锌。     

综合性无机化学实验:保健药品中钙、铁、锌含量的测定*

在大学无机化学实验教学中,应用元素含量测定技术,对营养保健药品中钙、铁、锌的含量进行定量测定,详细介绍了实验条件、测定方法和计算过程,并重点讨论了应用常规仪器对待测样品进行分离、纯化的方法和对干扰元素有效的掩蔽方法。通过对比实验结果与产品说明书中相关元素的含量数据,表明该实验方法具有较好的准确性和可操作性。     

Determination of selenium in blood serum by inductively coupled plasma atomic emission spectrometry with pneumatic nebulization

The possibility of determining selenium in blood serum using inductively coupled plasma emission spectrometry with conventional pneumatic nebulization was studied. A high-resolution spectrometer (SBW=6 pm) with laterally viewed ICP was employed. Analysis with conventional pneumatic nebulization could overcome laborious and demanding digestion, which is necessary for hydride generation. A pressure digestion with nitric acid at 160 degrees C was sufficient to decrease the carbon content in the serum sample to 5%-10% of its original value. Spectral interference of the CN band was observed and mathematically corrected. It was found that the carbon-induced selenium line emission enhancement occurred even under ICP optimized conditions. A method of determination was developed and applied to the analysis of blood serum. True limit of detection in real samples is 0.01-0.02 mg/L and the limit of quantification (RSD 10%) is 0.03-0.07 mg/L using Se I 196.090 nm line at an integration time of 10-2 s. The method was tested by analysis of porcine blood serum and the serum reference material Seronorm MI 0181.     

ICP-MS法测定聚酯纤维中TiO2含量

采用湿法和微波法对聚酯纤维样品进行消解,利用电感耦合等离子体质谱联用仪(ICP-MS)对样品中TiO2含量进行了测定,得到湿法消解样品测定值2 857.46μg/g(相对标准偏差为1.08%),微波消解样品测定值2599.21μg/g(相对标准偏差为2.76%).分别测定了两种消解方法的检出限,湿法消解检出限为4.0 ...     

Rapid characterization of protein chips using microwave-assisted protein tryptic digestion and MALDI mass spectrometry

We demonstrate that the microwave-assisted protein enzymatic digestion (MAPED) method can be successfully applied to the mass spectrometric characterization of proteins captured on the affinity surfaces of protein chips. The microwave-assisted on-chip tryptic digestion method was developed using a domestic microwave, completing the on-chip proteolysis reaction in minutes, whereas the previous on-chip digestion methods by incubation took hours of incubation time. For the model protein chips, antibody-presenting surfaces were prepared, where anti-α-tubulin1 and antibovine serum albumin (BSA) were immobilized on self-assembled monolayers. The resulting digestion efficiency, displaying sequence coverages of 30 and 14% for α-tubulin1 and BSA, respectively, was comparable to the previous time-consuming incubation studies. It allowed the characterization of immunosensed proteins by MASCOT search using peptide mass fingerprinting. In an example of this method for protein chip applications, BSA naturally involved in fetal bovine serum was unambiguously identified on a model protein chip by imaging mass spectrometry. This work shows that biomass spectrometry techniques can be implemented for surface mass spectrometry and biochip applications. Along with recent advances in imaging mass spectrometry, this technique will provide a new opportunity for high-speed, and thus high-throughput in the future, label-free mass spectrometric assays using protein arrays.     

电感耦合等离子体质谱(ICP-MS)法测定农产品地土壤中铅、镉、铬消解方法的改进

采用赶酸电热板消解农产品地土壤中的重金属,电感耦合等离子体质谱(ICP-MS)法同时测定土壤中的铅、镉、铬。研究了酸体系及酸用量、赶酸电热板的升温程序,确定了最佳消解条件。通过统计50个批次土壤样品中加入的质控样,做出质控图,结果表明:各元素测定值均落在中心附近、上下警告线之内,批次内平行样品各元素相对标准偏差均小于5%。方法克服了传统的电热板消解法的缺点,弥补了高压罐消解法和微波消解法的不足,方法快速、准确,适合于大批量样品的分析。     

Use of microwave digestion and atomic absorption spectrophotometry to determine chromic oxide as a digestibility marker in feed, feces, and ileal content.

Most conventional digestion procedures, such as dry ashing and wet ashing, are tedious and labor intensive. Microwave digestion is a good alternative, because microwave dissolution is faster, safer, and simpler, and provides more controlled reproducible conditions than conventional methods. The purpose of this study was to develop a microwave digestion method for mineralizing meat and bone meal diets, feces, and ileal contents. Each sample was heated on a hot plate for 10 min, dry ashed at 65 degrees C for 4 h, and transferred into microwave vessels. Then, 10 mL 70% HNO3 was added. Samples were digested for 7, 10, and 20 min at 95, 90, and 85% power, respectively. After the heating cycle, 6 mL 30% H2O2 was added, and samples were returned to the microwave for a second heating cycle of 1 and 7 min at 95% and 90% power, respectively. Finally, chromium concentration was determined by flame atomic absorption spectrophotometry. The digestion method was validated by using a standard reference material, SRM domestic sludge 2781, with a certified chromium value of 195 +/- 9 micrograms/g. The value obtained in this study was 178 +/- 11 micrograms/g, for a difference of 17 micrograms/g. Spike recovery experiments resulted in 103.16 and 100.35% recoveries of chromium from diet and feces samples, respectively. Coefficients of variation were 10.8 and 7.8%, respectively.     

原子荧光法测定土壤中砷的消解方法研究

分别用王水消解法和硫酸-硝酸-高氯酸混合酸消解法处理样品,用原子荧光光度计法测定了砷的含量,比较了两种消解方法砷的测定值和标准值.结果表明,采用混合酸消解法砷的测定值低于标准值,而采用王水消解法可以准确测定土壤中砷含量,实验操作简单方便,结果准确、可靠.     

酸对微波消解-氢化物发生原子荧光光谱法测定食品中锗的影响

以微波消解为前处理手段,采用氢化物发生原子荧光谱法测定食品中的锗,研究了作为载液的磷酸体积分数和消解过程中残留硝酸对测定结果的影响. 磷酸体积分数从5%增加至30%时,标准曲线斜率缓慢上升. 认为10%~20%体积分数磷酸适宜作为原子荧光光谱法测锗的载液. 硝酸在样品中体积分数超过1%后,锗的荧光信号严重减弱. 优化条件后对市售大蒜样品进行加标试验. 为进一步确定对有机锗的消解效果,对某批次锗-132胶囊进行测定. 大蒜加标试验回收率为109.7%,胶囊测定值为标签标识值的81.4%. 两次试验结果均较为满意,说明方法具有可靠性.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定ADC12中硅

在微波消解仪中以氢氧化钠溶解试样,然后滴加过氧化氢,使得铸造铝ADC12中的硅完全溶解,并采用电感耦合等离子体原子发射光谱(ICP-AES)法测定,硅的质量百分数平均值为10.31％的情况下,标准偏差0.09％,相对标准偏差(RSD)为0.83％.对比了国家标准方法中加热板消解法与微波消解法对硅加标回收率的影响,加热板消解法的加标回收率低于微波消解法,微波消解法辅助前处理样品,促使样品在短时间内反应完全,实验步骤简便,结果满意.     

Analysis of human serum by liquid chromatography-mass spectrometry: improved sample preparation and data analysis

Discovery of biomarkers is a fast developing field in proteomics research. Liquid chromatography coupled on line to mass spectrometry (LC-MS) has become a powerful method for the sensitive detection, quantification and identification of proteins and peptides in biological fluids like serum. However, the presence of highly abundant proteins often masks those of lower abundance and thus generally prevents their detection and identification in proteomics studies. To perform future comparative analyses of samples from a serum bank of cervical cancer patients in a longitudinal and cross-sectional manner, methodology based on the depletion of high-abundance proteins followed by tryptic digestion and LC-MS has been developed. Two sample preparation methods were tested in terms of their efficiency to deplete high-abundance serum proteins and how they affect the repeatability of the LC-MS data sets. The first method comprised depletion of human serum albumin (HSA) on a dye ligand chromatographic and immunoglobulin G (IgG) on an immobilized Protein A support followed by tryptic digestion, fractionation by cation-exchange chromatography, trapping on a C18 column and reversed-phase LC-MS. The second method included depletion of the six most abundant serum proteins based on multiple immunoaffinity chromatography followed by tryptic digestion, trapping on a C18 column and reversed-phase LC-MS. Repeatability of the overall procedures was evaluated in terms of retention time and peak area for a selected number of endogenous peptides showing that the second method, besides being less time consuming, gave more repeatable results (retention time: <0.1% RSD; peak area: <30% RSD). Application of an LC-MS component detection algorithm followed by principal component analysis (PCA) enabled discrimination of serum samples that were spiked with horse heart cytochrome C from non-spiked serum and the detection of a concentration trend, which correlated to the amount of spiked horse heart cytochrome C to a level of 5 pmol cytochrome C in 2 microl original serum.     

微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定高速工具钢中锰、磷、镍、铜、铬、钒

高速工具钢为高碳高合金工具钢,常温下样品酸溶分解较为困难,因此建立了微波消解电感耦合等离子体原子发射光谱法(ICP-AES)测定高速工具钢中锰、磷、镍、铜、铬、钒的方法,利用微波消解提高溶样的温度和压力,在王水、氢氟酸和硫酸介质中使样品充分消解,再用饱和硼酸溶液络合过量的氢氟酸,基体匹配消除铁基体的影响,ICP-AES法同时测定锰、磷、镍、铜、铬、钒的含量。测定高速工具钢标准样品,测定值与标样值相吻合,方法的相对标准偏差在0.55%~4.1%。加标回收率在95.6%~114.8%,满足测定要求。