Studies on the persistence of estradiol benzoate and nortestosterone decanoate in hair of cattle following treatment with growth promoters,determined by ultra-high-performance liquid chromatography–tandem mass spectrometry

Measurement of steroid esters in bovine hair samples, using sensitive liquid chromatography-tandem mass spectrometry (LC–MS/MS), provides a powerful tool for identifying animals treated illicitly with growth promoters. The successful application of such testing requires appropriate sampling of hair from treated animals. This paper describes the results of hair analysis by LC–MS/MS for two animal studies in which animals were treated with estradiol-3-benzoate and nortestosterone decanoate. The results from the first animal study indicate that animals treated with these anabolic steroids may not always be identified from analysis of hair samples; positive test results occur sporadically and only for some of the treated animals. The results from the second animal study identify conditions attaching to positive hair samples, such as, that concentrations of steroid esters in hair are related to distance of sampling from point of injection and to time post-treatment, that concentrations of steroid esters in hair are related to dose given to the animal but that this relationship may vary over time post-treatment, and that steroid esters may be measured in regrowth hair taken some weeks after treatment. Steroid esters are determined along the length of the hair, confirming that accumulation of steroid esters into hair occurs from various sources, including blood, sweat and sebum. The reported research provides some useful insights into the mechanisms governing the persistence of steroid esters in bovine hair following illicit treatment with growth promoters.     

Hollow fiber liquid phase microextraction combined with electrothermal atomic absorption spectrometry for the speciation of arsenic (III) and arsenic (V) in fresh waters and human hair extracts

A new method of hollow fiber liquid phase microextraction (HF-LPME) using ammonium pyrrolidine dithiocarbamate (APDC) as extractant combined with electrothermal atomic absorption spectrometry (ETAAS) using Pd as permanent modifier has been described for the speciation of As(III) and As(V). In a pH range of 3.0-4.0, the complex of As(III)-APDC complex can be extracted using toluene as the extraction solvent leaving As(V) in the aqueous layer. The post extraction organic phase was directly injected into ETAAS for the determination of As(III). To determine total arsenic in the samples, first As(V) was reduced to As(III) by l-cysteine, and then a microextraction method was performed prior to the determination of total arsenic. As(V) assay was based on subtracting As(III) form the total arsenic. All parameters, such as pH of solution, type of organic solvent, the amount of APDC, stirring rate and extraction time, affecting the separation of As(III) from As(V) and the extraction efficiency of As(III) were investigated, and the optimized extraction conditions were established. Under optimized conditions, a detection limit of 0.12 ng mL⁻¹ with enrichment factor of 78 was achieved. The relative standard deviation (R.S.D.) of the method for five replicate determinations of 5 ng mL⁻¹ As(III) was 8%. The developed method was applied to the speciation of As(III) and As(V) in fresh water and human hair extracts, and the recoveries for the spiked samples are 86-109%. In order to validate the developed method, three certified reference materials such as GBW07601 human hair, BW3209 and BW3210 environmental water were analyzed, and the results obtained were in good agreement with the certified values provided.     

2,4-二硝基氟苯柱前衍生高效液相色谱法测定18种氨基酸

建立了测定18种氨基酸的高效液相色谱方法。以Hypersil ODS-c_(18)柱(100mm×4.6mm i.d.,5μm)为色谱柱,2,4-二硝基氟苯为衍生化试剂,梯度洗脱。流动相A:0.05mol/L乙酸钠缓冲溶液(pH=6.5,含10mL/LN,N-二甲基甲酰胺),流动相B:乙腈-水(体积比为1:1)。所测氨基酸组分的浓度在0.2～3.0mg/L范围内与峰面积之间具有良好的线性关系,回收率为90.4％～101.0％,检出限为0.120～1.225mg/L,测定结果的相时标准偏差为1.05％～5.93％。     

Generation of anti-azoxystrobin monoclonal antibodies from regioisomeric haptens functionalized at selected sites and development of indirect competitive immunoassays

Azoxystrobin is a modern strobilurin fungicide used around the world to combat prime diseases affecting highly valuable crops. Accordingly, residues of this chemical are frequently found in food, even though mostly under maximum tolerated levels. We herein describe the development of an indirect competitive immunoassay for the determination of azoxystrobin residues. A panel of monoclonal antibodies displaying subnanomolar affinity to azoxystrobin was generated using, as immunizing haptens in mice, four functionalized derivatives carrying the same spacer arm located at different rationally chosen positions. This collection of antibodies was thoroughly characterized with homologous and heterologous antigens, and the immunoassay consisting of monoclonal antibody AZo6#49 and the coating conjugate OVA–AZb6, which displayed an IC₅₀ value of 0.102 μg L⁻¹ and a LOD of 0.017 μg L⁻¹, was eventually optimized. The response to different pH and ionic strength conditions of the specific assay was studied using a biparametric approach. In addition, the influence of Tween 20 and organic solvents over the assay parameters was also evaluated. After optimization, the developed immunochemical assay was applied to the analysis of azoxystrobin in spiked juices of relevant fruits and vegetables, showing excellent recoveries between 2 and 500 μg L⁻¹.     

汉中市三组年龄段人群发 Pb含量测定分析

用原子吸收光谱法测定了健康少儿、青年、中老年三个年龄段共 2 74人发Pb含量。统计结果表明 ,中老年组发Pb含量最高 ( 9 52 1× 1 0 - 6 ± 2 3 3 9× 1 0 - 6 ) ,三组发Pb有明显差异。各组男女之间发Pb含量无显著性差异 ,Pb与Cd、Fe有相关性。提示当某些必需元素随着年龄增长而降低时 ,发Pb却有随着年龄增长而增高的倾向 ,故Pb在体内的蓄积作用对中老年人带来的危害更应受到关注     

对乙酰基偶氮胂吸光光度法测定微量铜

在pH5.0的(CH2)6N4-HCl缓冲介质中,Cu(Ⅱ)与对乙酰基偶氮胂(ASApA)形成1比2络合物,λmax＝598nm,εmax=1.30×104L·mol-l·cm-1,铜浓度在0～2.0mg·L-1范围内遵从比耳定律。方法用于粮食、食品、水、树叶及人发等试样中铜的测定,结果满意。     

幼儿头发中微量元素含量与身高、体重关系研究

普查了４４９名１－６岁儿童头发中锌、铁、铜、钙、锰、铅含量,用分层聚类分析法对其身高、体重与各元素进行相关分析。幼儿身高与头发中锌含量呈相关关系,与头发中铅含量呈负相关关系。体重与头发中锌含量呈显著的正相关关系。与头发中铅含量呈负相关关系。说明锌有利于身体发育,而铅对身体发育不利。     

幼儿头发中微量元素含量相关性研究

为探讨儿童头发中微量元素是否有协同或拮抗作用,测定了646名1－3岁和3803名4－7岁儿童头发中的Zn,Fe,Cu,Ca,Mn和Pb含量,并研究了各元素间的相互关系,结果表明：1－3岁幼儿头发中Zn,Fe,Cu,Ca,Mn和Pb各元素间均呈正相关,4－7岁儿童的发锌含量与发铅含量呈非常显著负相关（P值均＜0．001）,其它各元素间均呈正相关。     

中山市火炬开发区1078例儿童头发微量元素临床研究

为了探讨微量元素对儿童健康的影响,检测了中山市火炬开发区1078名2个月－14岁儿童头发锌,锌,铜,钙,锰,铅,结果发现,不同年龄儿童同一元素的含量不同,婴,幼儿组发锌,铁,钙明显低于其他年龄组,同时缺锌,缺铁,铁钙,高铅是引起儿童厌食,佝偻病, 呼吸道感染的主要原因,建议针对病因开展儿童微量元素缺乏的防治工作。     

头发锌含量测定的应用价值评价

以114例2－5岁儿童为对象，同时取其末梢血和头发，测定锌含量。以全血锌值为标准，评价头锌测定的应用价值。结果显示，头发锌测定的灵敏度可达86．1％，特异度为52．4％，符合率为73．7％。