血清中锂的原子吸收法测定

对血清中锂的火焰原子吸收分光光度分析法（ＦＡＡＳ）进行了研究，发现血清在０．２４ｍｏｌ／ＬＨＮＯ３介质中，用３０００×１０－６Ａｌ３＋作为碱土金属干扰的抑制剂，用ＦＡＡＳ法测定血清理，其回收率和精密度都很好，分别为１０４．７％和２．８％．本法１％吸收的灵敏度为０．０３３μｇ／ｍＬ。采用本法对服用碳酸锂治疗苯中毒的患者血清中锂进行了测定，其含量在０．７５～４．６４μｇ／ｍＬ之间，结果令人满意。     

火焰原子吸收光谱法间接测定非金属材料中氯

报道了火焰原子吸收光谱法（ＦＡＡＳ）间接测定非金属材料中氯的方法，采用ＡｇＣｌ沉淀，测定剩余Ａｇ~＋间接求出氯含量。方法的特征浓度为０．０１４ｍｇ／Ｌ（１％吸收），检出限为０．０３２ｍｇ／Ｌ（３），测定下限为０．１１ｍｇ／Ｌ，相对标准偏差（ＲＳＤ）为１．５％～１０％，样品加标准回收率在９１．４％－１０５％之间。     

反相HPLC测定钒,铌,钽的2—（2—吡啶偶氮）—5—二乙氨基苯酚配合物

以２－（２－吡啶偶氮０－５－二乙氨基苯酚（ＰＡＤＡＰ）为柱前衍生试剂，在含０．１％酒石酸的１０ｍｍｏｌ／Ｌ（ｐＨ３．５）ＨＡｃ－ＮａＡｃ缓冲溶液的甲醇／水（５０∶５０，Ｖ／Ｖ）中（５８０ｎｍ检测），在Ｃ１８柱上于１１ｍｉｎ内实现了Ｖ、Ｎｂ、Ｔａ的同时分离及测定，检出限（Ｓ／Ｎ＝３）杰０．３４、０．２９、７．３０ｎｇ／ｍＬ．该法灵敏度高，用于矿样分析所得民推荐值相行，标准加入回收率为９９．０％～１０     

芦荟大黄素的电化学研究

用单扫示波极谱法研究了芦荟大黄素的电化学行为。在５％Ｎａ２ＣＯ３＋５％ＮａＯＨ（９＋１）底液中，芦荟大黄素于－０．８４Ｖ（Ｐ１）和－０．９７Ｖ（Ｐ２）处产生两个示波极谱峰，利用Ｐ１可测定芦荟大黄素，线性范围为 ０．１１－２４ｍｇ／Ｌ和３．０－２８．６ｍｇ／Ｌ，检测限为０．０６ｍｇ／Ｌ。将该法应用于中药大黄中的芦荟大黄素的测定，结果满意。另外，讨论了芦荟大黄素清除由邻苯三酚自氧化产生的超氧自由基（Ｏ２）的作用。     

液相色谱法测定生物发酵液中水溶性维生素的研究

本文采用反相离子对色谱测定了生物发酵液中的七种水溶性维生素。提出了用自行装填的酸性氧化铝（０．１９～０．１５ｍｍ）前置柱，和５％乙酸洗脱样品的前处理方法；并就有关的色谱条件进行了选择。色谱柱为ＮｏｖａＰａｋＣ１８；流动相Ａ液为０．０５ｍｏｌ／Ｌ庚烷磺酸盐（ＰＩＣＢ７），冰乙酸调ｐＨ＝２．５；Ｂ液为甲醇＋三乙胺（１００＋０．５）；梯度洗脱；ＵＶ２５４ｎｍ、２９０ｎｍ、３６０ｎｍ同时测定。线性范围为０．１～１０μｇ，各种维生素的ＲＳＤ在１．２％～３．０％之间（ＶｉｔａｍｉｎＢ１２除外），回收率大于９０％。     

不经分离,高敏,连续光度滴定混合物中钕和铁

提出以Ｆｅ（３＋）（Ｎｄ（３＋）－ＣＡＳ－ＣＰＢ－Ｃ２Ｈ５ＯＨ作为不经分离、高敏、连续光度配合滴定混合物中Ｆｅ（３＋）和Ｎｄ（３＋）的多元胶束配合指示体系。滴定Ｆｅ（３＋）和Ｎｄ（３＋）的适宜ｐＨ分别为２．３～３．２和６．０～８．６。用ＥＤＴＡ目视滴定Ｆｅ（３＋）时，终点处由蓝紫变粉红色，对比度大（Δλ＝１３０ｎｍ）、灵敏度高（配合物摩尔吸光系数ε（６３０）＝１．１４×１０５Ｌ·ｃｍ（－１）·ｍｏｌ（－１），至少可检测０．４μｇ／ｍＬ，滴定线性范围为０～２．８μｇ／ｍＬ。线性相关系数为０．９９９４；目视滴定Ｎｄ（３＋）时，终点处由绿色变橙黄，Δλ＞１８０ｎｍ，ε（６３０）＝７．６×１０４，至少可检测１μｇ／ｍＬ，滴定线性范围０～３．７μｇ／ｍＬ，线性相关系数０．９９９４。对于铁钕硼混合物样品则不经分离在６３０ｎｍ处连续光度滴定，可更精密、高敏、准确地确定终点，变异系数１．７６％～２．８６％，标准加入回收率９６％～１０４％，且简便、快速。     

病人血样中痕量锗,锶的石墨炉原子吸收光谱法测定

本文运用石墨炉ＡＡＳ法加基体改进技术，测定了５０岁以上病人血清及环境水样中锗和锶的含量。用０．０１ｍｏｌ／ＬＨＮＯ３－０．１％ＴｒｉｔｏｎＸ－１００稀释血清，测定精度可与火焰法媲美。锗，锶的特征量分别为２８ｐｇ和１８ｐｇ；线性范围为０－２５０ｎｇ／ｍＬ和－３５．０ｎｇ／ｍＬ；相对标准偏差（ｎ＝１０）４．１０％和２．４９％；回收率分别为９２．２％－９９．０％和９２．０％１０２％。方法快速准确，结果满     

Raney Cu催化剂制备规律的研究Ⅰ.碱抽提动力学模型建立

恒压下,跟踪测定析氢体积（Ｖ）,考察了氢氧化钾水溶液与Ｃｕ２７．１Ａｌ７２．９合金反应的动力学。在实验结果的基础上,提出了理想模型,并推导出了下述机理型动力学式：ｍｑｔ＝－（１／３）ｌｎ「（１＋ｑＲ１）／（１＋ｑＲ０）」＋（１／６）ｌｎ（「（ｑＲ１）＾２－（ｑＲ１）＋１」／「ｑＲ０）＾２－（ｑＲ０）＋１」）－（１√ｅ）（ａｒｃｔｇ「２√３）（ｑＲ１－１√２）」－ａｒｃｔｇ「（２√３）（ｑＲ０－１／     

反相高效液相色谱法测定食品中水溶性维生素的含量

采用反相色谱法同时测定食品中水溶性维生素（Ｖｉｔａｍｉｎ）Ｃ、Ｂ５、Ｂ６、Ｂ１、Ｂ２和Ｂ１２的含量，ＰＣ８１０／Ｓ２５０４（４．０ｍｍ×２５０ｍｍ，１０μｍ）柱，０．１ｍｏｌ／Ｌ甲酸铵甲酸溶液（ｐＨ＝４．５，含０．４％二乙胺）＋甲醇（７５＋２５）为流动相，流速１ｍＬ／ｍｉｎ，ＵＶ２５４ｎｍ，１２ｍｉｎ内实现了良好分离，乙酰苯胺为内标物。苹果及强化奶粉中维生素平均回收率分别为９２．５０％～１０５．６０％和９５．００％～１０２．８０％，该法操作简便、迅速、可靠、测试费用低。     

沉淀滴定法测定碘

提出沉淀滴定Ｉ－的新方法，以聚乙烯醇（ＰＶＡ）作为沉淀的胶体保护剂，（Ｉ）－３（碘钅翁离子）作为吸附指示剂，用ＡｇＮＯ３标准溶液直接测定Ｉ－；讨论了滴定机理。检测范围为０．０１～０．１ｍｏｌ／Ｌ，相对误差小于０．２％。本法已用于鸡饲料添加剂中Ｉ－的测定。     

新生儿脐血清微量元素测定及与生长发育关系研究

应用电感耦合等离子体发射光谱法测定也３３名新生儿脐血清中１７种微量元素（铁、铜、锰、锌、钴、钼、硒、铬、锡、钒、硅、镍、镉、铅、锶、钛、铝）及３种常量元素（钙、磷、镁）的含量。结果表明,新生儿脐血清微量元素性别分布接近,仅女婴血清铬、钒高于男婴,但地区差异明显,城镇新生儿脐血清中锰、锌、锶、钛、钙较高,而钼、硒、铬、铝较低。多元回归分析显示,血清元素铁、锰、锌、硒、硅、锶、钙被引人新生儿体重和发育     

Quantification of myo‐inositol, 1,5‐anhydro‐ D‐sorbitol,and D‐chiro‐inositol using high‐performance liquid chromatography with electrochemical detection in very small volume clinical samples

Inositol is a six‐carbon sugar alcohol and is one of nine biologically significant isomers of hexahydroxycyclohexane. Myo‐inositol is the primary biologically active form and is present in higher concentrations in the fetus and newborn than in adults. It is currently being examined for the prevention of retinopathy of prematurity in newborn preterm infants. A robust method for quantifying myo‐inositol (MI), D ‐chiro‐inositol (DCI) and 1,5‐anhydro‐ D ‐sorbitol (ADS) in very small‐volume (25 μL) urine, blood serum and/or plasma samples was developed. Using a multiple‐column, multiple mobile phase liquid chromatographic system with electrochemical detection, the method was validated with respect to (a) selectivity, (b) accuracy/recovery, (c) precision/reproducibility, (d) sensitivity, (e) stability and (f) ruggedness. The standard curve was linear and ranged from 0.5 to 30 mg/L for each of the three analytes. Above‐mentioned performance measures were within acceptable limits described in the Food and Drug Administration's Guidance for Industry: Bioanalytical Method Validation. The method was validated using blood serum and plasma collected using four common anticoagulants, and also by quantifying the accuracy and sensitivity of MI measured in simulated urine samples recovered from preterm infant diaper systems. The method performs satisfactorily measuring the three most common inositol isomers on 25 μL clinical samples of serum, plasma, milk, and/or urine. Similar performance is seen testing larger volume samples of infant formulas and infant formula ingredients. MI, ADS and DCI may be accurately tested in urine samples collected from five different preterm infant diapers if the urine volume is greater than 2–5 mL. Copyright © 2015 John Wiley & Sons, Ltd.     

急性脑血管病患者血清元素的测定

采用高频等离子体发射光谱法测定了３４例脑梗塞、３３例脑出血和对照组２７人血清锌、铜、锰、铬、镁、钼、锶、铁、钛、钡、镉和钙共１２种元素的含量。结果显示脑梗塞和脑出血组血清锌和锌／铜比值显著高于对照组；锰和钼含量仅在脑梗塞组明显增高，锶仅在脑出血组显著增高，而其它几种元素疾病组与对照组无显著性差异。伴有高血糖、高血脂和高血压的病人，其血铬含量显著降低，表明锌、锌／铜比值、锰、钼、锶、铬元素与急性脑血     

环形聚焦单模微波消解–ICP–MS法检测罐头食品中钒、铬、镍、镉、铅、砷、锰、铝、铜、锡

建立环形聚焦单模微波消解–电感耦合等离子体质谱法同时测定罐头食品中钒、铬、镍、镉、铅、砷、锰、铝、铜、锡金属元素的含量。采用浓硝酸消解样品,各元素分析目标物分别为Pb208,Cd111,As75,Mn55,Cu63,V51,Ni60,Sn120,Cr53,Al27。Pb208以Bi209为内标,Cd111,Sn120以In115为内标,Ni60,Cr53,V51,Mn55,Cu63,As75,Al27以Sc45为内标。各元素工作曲线线性良好,相关系数不小于0.999 5,方法检出限为0.0030~0.030μg/g,加标回收率在98.0%~104.1%之间,测定结果的相对标准偏差为1.29%~4.50%(n=6)。该方法简便快捷,灵敏度高,适合分析大批量罐头食品中多种金属元素。     

电感耦合等离子体-发射光谱法（ICP-AES）快速测定饮用水中8种微量元素

用电感耦合等离子体-发射光谱法（ICP-AES）同时快速测定饮用水中微量的铜、铅、锌、铁、锰、镉、铬、砷,具有快速、简便、灵敏度高等优点,精密度为1．2％～8．2％（RSD,n=5）．回收率为90％～110％．     

Ultra high performance liquid chromatography coupled to tandem mass spectrometry determination of lipid peroxidation biomarkers in newborn serum samples

Byproducts of arachidonic (AA) and docosahexaenoic acid (DHA) oxidation are highly relevant for the study of free radical associated conditions in the perinatal period. Plasma metabolites can provide the clinician with a snapshot of the oxidant status of patients before and after specific clinical interventions (e.g.: supplementation with oxygen). We describe a new andreliable ultra-performance liquid mass spectrometry method to determine F2-isoprostanes and other byproducts (isoprostanes, isofurans, neuroprostanes, neurofurans) in newborn serum samples. Cord blood samples were obtained from severely depressed newborn infants (Apgar score 1 min < 3; arterial cord pH < 7.00), and aliquoted for serum determination and stored at −80 °C. A UHPLC-MS/MS method was employed. It has a series of technical advantages: simple sample treatment; reduced sample volume (100 μL) which is essential for preterm neonates with low circulating blood volume, high throughput of sample analysis (96 samples in less than 24 h) and high selectivity for different isoprostanes isomers. Excellent sensitivity was achieved within limits of detection between 0.06 and 4.2 nmol L⁻¹, which renders this method suitable to monitoranalyte concentration in newborn samples. The method's precision was satisfactory; with coefficients of variation around 5–12% (intra-day) and 7–17% (inter-day). The reliability of the described method was assessed by analysis of spiked serum samples obtaining recoveries between 70% and 120%. The proposed method has rendered suitable for serum determination for newborn babies at risk of oxygen free radical associated conditions.     

Biomonitoring of occupational exposure: Neutron activation determination of selected metals in the body tissues and fluids of workers manufacturing stainless steel vessels

Occupational exposure was examined for 20 workers dealing with welding, polishing, and assembling of stainless steel vessels. Instrumental neutron activation analysis was used for determination of selected elements in hair and nail, whereas urinary Cr and Mn, blood Mn and serum Cr were determined by radiochemical neutron activation analysis. Increased levels of Cr in hair, nails, serum and urine, Mo in hair, and Mn in blood were found in the exposed group compared to controls. Accuracy of the results was proven by analysis of reference materials and by comparison of element levels in controls with reference values for non-exposed persons.     

Microwave assisted digestion of atmospheric aerosol samples followed by inductively coupled plasma mass spectrometry determination of trace elements

A microwave digestion method in a closed vessel was developed for the determination of trace metals in atmospheric aerosols using inductively coupled plasma mass spectrometry (ICP-MS). A recovery study for the elements V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Cd, Sb, and Pb was conducted using multi-elemental standard solutions, NIST 1633b Trace Elements in Coal Fly Ash, and NIST 1648 Urban Particulate Matter. A simple digestion method using only HNO3/H2O2 gave good recoveries (90%-108%) for all elements except Cr in SRM 1648, but yielded low recoveries for SRM 1633b. A more robust method using HNO3/H2O2/HF/H3BO3 yielded higher recoveries (82%-103%) for the lighter elements (V-Zn) in SRM 1633b, and improved the Cr recovery in SRM 1648, but decreased the Se recovery in both SRMs. A comparative analysis of aerosol samples obtained at a remote mountain location Nathiagali, Pakistan (2.5 km above mean sea level), and Mayville, New York, downwind from the highly industrialized Midwestern United States, was carried out using Instrumental Neutron Activation Analysis (INAA) for the elements Cr, Mn, Fe, Co, Zn, As, Se, and Sb. The simple digestion method yielded excellent agreement for Cr, Fe, Zn, As, Se, and Sb, with slopes of the ICP-MS vs. INAA regressions of 0.90-1.00 and R2 values of 0.96-1.00. The regressions for Mn and Co had slopes of 0.82 and 0.84 with R2 values of 0.83 and 0.82, respectively. Addition of HF/H3BO3 did not improve the correlation for any of the elements and degraded the precision somewhat. The technique provides sensitivity and accuracy for trace elements in relatively small aerosol samples used in atmospheric chemistry studies related to SO2 oxidation in cloud droplets. The ability to determine concentrations of a very large number of elements from a single analysis will permit source apportionment of various trace pollutants and hence strategies to control the sources of air pollution. This is particularly important as the health effects of particulate matter are increasingly recognized.     

Trace element analysis of human blood serum by neutron activation analysis

An attempt was made to see if there is any correlation between the trace element concentrations in the human blood serum and some specific disease. The serum samples of the patients suffering from cancer, Down syndrome, and Banti syndrome were analyzed by the neutron activation method and compared with the trace element concentrations observed among the clinically healthy men. The cancer patients gave below normal concentrations in Rb, Mn, Fe, Co, Cu, Zn, Al and Se. The Down syndrome patients were found to have similar deficiencies in Cr, Mn, Fe, Co, Zn, Cu and Sb.     

Radiochemical separations for inorganic trace elements in some biological reference materials,foods, tissues and body-fluids

A simple radiochemical machine incorporating ion-exchange procedures has been described. The system has been tested repeatedly for the determination of Cd, Co, Cr, Cu, Mn and Mo at ultra trace concentration levels in a variety of biological samples such as reference materials, human blood serum, human milk, hair and certain dietary materials, thereby demonstrating its suitability for practical use. The procedure can also yield results for A, Au and W, without any further chemical manipulations. Results show <1, 0.12, 0.18, 983, 0.61 and 0.91 g/l for Cd, Co, Cr, Cu, Mn and Mo, respectively, in human blood serum. Corresponding concentrations in human milk are <1, 0.25, <1, 186 to 310, 4 to 40 and 5.8 g/l. Among the reference materials, IAEA milk standard A-11 shows 1.85, 5.1, 17, 380, 260 and 101 ng/g for Cd, Co, Cr, Cu, Mn and Mo, respectively. Corresponding concentrations in animal muscle H-4 are 4.1, 5, 10.2, 4000, 455 and 45 ng/g. Importantly, this scheme has been applied to process large number of samples from single investigations such as those arising from dietary studies, obtaining quick and reliable data for routine use.In memory of Knut Samsahl, the devoted Norwegian radiochemist.