液相色谱法测定血中巴比妥类药物

本文建立了血样中巴比妥类药物的液相色谱定性定量分析方法，该法采用Ｃ１８反相色谱柱分离，二极管矩检测器检测，能一次性将４种药物分析和鉴定，通过色谱峰的保留时间和紫外吸收光谱定性，以色谱的峰面积定量，标准曲线的直线范围在０－１０μｇ．ｍ１＾－１，相关系数在０．９９以上。血中药物经溶浏萃取，回收率在９５％以上，血中的杂质不影响药物检测。方法的最小检出浓度为１０ｎｇ．ｍ１＾－１，本法可用于临床中毒样品的分     

头发中多种新型有机污染物检测方法的建立

本研究基于超声提取-分散固相萃取技术，建立了同时分析头发中多溴联苯醚(PBDEs)、有机磷系阻燃剂(OPFRs)、全氟及多氟烷基化合物(PFASs)、邻苯二甲酸酯(PAEs)及其代谢物(mPAEs)等5类有机污染物的前处理方法.头发样品(0.1 g)研磨成粉/絮状后经4 mL正己烷:丙酮:乙酸乙酯:乙腈(1:1:1:1,V/V/V/V)混合溶液提取3次，加入20 mg无水硫酸钠(Na₂SO₄)和100 mg十八烷基硅烷键合硅胶(C18)净化除杂，氮吹浓缩后分别采用GC-MS、GC-MS/MS和LCMS/MS进行分析.实验采用内标法定量，所有目标化合物在其相应的质量浓度范围内线性关系良好，相关性系数大于0.995;5类化合物检出限介于0.042—364.7 ng·g^-1，加标回收率在53.6%—138%之间，相对标准差及日内/间精密度均小于20%.采用该方法对广州市10例男性头发进行了检测，所有样品均检出全氟辛烷磺酸(PFOS)、邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二...     

污水处理厂中微塑料的分析方法研究进展

随着研究的深入,微塑料在世界各地的污水处理厂中的赋存特征及潜在影响已逐渐成为新的研究热点,而研发适用性强、重复性高的提取鉴定方案是重要前提.当前,污水处理厂样品的复杂性导致现有微塑料的提取及鉴定方法多种多样.本文对现有的样品采集(大样本法与浓缩样本法)、预处理(消解及分离方法)和鉴定方法(目视法、光谱法及热分析法)进行了系统梳理和对比分析,以期为今后污水处理系统中微塑料的相关研究提供帮助.     

发光细菌法检测环境污染中的基因毒性

用明亮发光杆菌Ｔ３小种的暗变种Ｔ９１７１菌株检测９种化合物和１４种环境样品的基因毒性。结果表明，在９种化合物中检出３种阳性物，６种可疑物。在１４种环境样品中检出２个样品呈阳性，７个样品呈可疑，其余为阴性。激活系统Ｓ９能极大地提高试验的灵敏度。在环境基因毒物的筛选中，发光细菌法是一种非常有价值的短期生物试验方法。表２参１４     

稻米中农药敌枯双降解物的高效液相色谱测定法

本文提出了一种分析在稻米中的农药敌枯双降解物敌枯唑的高效液相色谱法。样品用丙酮提取,经氧化铝柱层析净化后,以氨基键合固定相,氯伤-乙醇-二甲基甲酰胺为流动相,紫外检测器测定,外标法定量。方法平均回收率为84％,最低检出浓度为0.003ppm。用提出的方法分析了田间施药的稻米样品13个。     

固相萃取法提取净化生物检材中三类农药的实验研究

本文以常见的六种有机磷类、四种氨基甲酸脂类和五种拟种虫菊酯类农药为对象，研究了用国产ＧＤＸ－４０３或Ｃ１８固相小柱同时提取净化环境样品和生物检材中三种类型的农药，分别采用ＧＣ／ＦＰＤ，ＧＣ／ＮＰＤ和ＧＣ／ＥＣＤ三种特征性气相色谱法进行分析鉴定，为系统分析有机农药提供了一套快速、简便的固相提取方法。     

分散固相萃取-气相色谱/质谱联用法测定水稻中嘧菌酯和戊唑醇含量

建立了简便、高效、同时测定水稻中嘧菌酯和戊唑醇两种不同类型杀菌剂的检测方法,对比了几种常用的提取溶剂和不同的提取方法之间的回收率和净化效果,选择了分散固相萃取作为样品前处理方法.采用GC-MS-SIM方法进行检测,外标法定量,为水稻中嘧菌酯和戊唑醇的分离测定提供了有效可行的方法,相对于当前较多使用的液相色谱-质谱检测方法节省了时间和检测成本.结果表明,嘧菌酯在0.002—2.5μg·mL-1质量浓度范围内呈良好线性关系,最小检出量为0.002 ng,在稻米、稻壳和植株的最低检出浓度分别为0.008、0.016、0.016 mg·kg-1;戊唑醇在0.001—2.5μg·mL-1质量浓度范围内呈良好线性关系,最小检出量为0.001ng,在稻米、稻壳和植株的最低检出浓度分别为0.004、0.008、0.008 mg·kg-1.在稻米、稻壳、植株中分别进行了3个水平的添加回收实验,戊唑醇的平均添加回收率为78.9%—104.3%,相对标准偏差为1.4%—6.0%;嘧菌酯的平均添加回收率为86.9%—104.0%,相对标准偏差为1.5%—7.5%.     

提取土壤中23种有机氯农药:微波法与索氏法对比

本文研究了微波辅助提取土壤中23种有机氯农药的提取效果，并与传统的索氏提取方法作了系统对比．另外，对采集于河北省某地污灌土壤的样品进行两种方法提取效率的对比分析．     

多氯联苯中氯代二苯并二噁和氯代二苯并呋喃分析

采用GC/MS法对国产PCBs中的PCDDs和PCDFs进行了成分鉴定.样品溶于石油醚中,经两次氧化铝柱分离以消除干扰物质,然后用选择离子GC/MS法进行PCDDs和PCDFs的定性、定量分析.在PCB_5中检出了三至八氯取代的PCDFs,但在PCB_3中只发现了三至六氯取代的PCDFs.两种样品中都检出了剧毒的2,3,7,8-TCDD化合物.与国外产品相比,国产PCBs中不仅含有较高量的PCDFs还含有PCDDs.     

生物样品中氯苯类化合物的提取和测定

以水草和鱼样品为研究对象,采用超声波法提取生物样品中的氯苯类化合物(CBS)并用气相色谱进行定性和定量分析.结果表明:用超声波提取生物样品中CBS的最佳提取溶剂为正己烷,功率为25W,提取时间为20 min.植物和动物样品中CBS的提取方法稍有不同.在最佳提取条件下,鱼样中的平均加标回收率为75.2%～91.6%,水草中的平均加标回收率为88.2%～94.3%.另外,要根据污染物的检出限,确定生物样品中污染物提取的浓缩倍数.结论:用超声波法提取生物样品中的CBs的方法是可行的.     

Lead,cadmium, copper,zinc, iron,and calcium in human hair as a function of gender,age, smoking,and hair dyeing

Hair samples were collected randomly from 110 subjects (55 male and 55 female) ranging in age from (<15–60) years. Each subject was asked to complete a personal questionnaire describing his/her sex, age, general health, smoking, use of hair dyes, occupational area, and living habits. Concentrations of Pb, Cd, Cu, Zn, Fe, and Ca in human hair samples were evaluated using atomic absorption spectrometry. Results indicated that concentrations of Pb, Cd, Cu, and Zn in the hair of smokers were higher than those in the hair of non-smokers, whereas, Fe and Ca concentrations in hair of smokers were lower than those in hair of non-smokers. Moreover, the concentrations of these elements are higher in dyed hair compared with undyed hair.     

Increase in Hair Lead, but not Blood Lead Content of Occupationally-Exposed Workers

This study attempted to investigate whether increased hair lead concentrations due to environmental exposure are accompanied by parallel increases in blood lead concentrations. A sample set consisting of both occupationally-exposed individuals and persons from the general population was investigated. The lead content of scalp and pubic hair from the general population (n=189), traffic police personnel (n=27) and battery workers (n=22) were analysed. The hair samples were taken from the nape of the neck by cutting 23 cm closest to the scalp and cleaned using a washing procedure developed in our laboratory. The effectiveness of the washing procedure was partly determined by examining the scanning electron micrographs of the hair samples. Venous samples of blood were taken from each volunteer's arm.The traffic police and battery plant operators sampled had significantly higher average scalp hair and pubic hair lead levels than the non occupationally-exposed general population. No significant differences were found between the blood lead values of these workers and the general population. Compared to the general population both occupationally-exposed groups had significantly more symptoms of lead toxicity.Lead particles were still observed on the hair shafts after the washing procedure. The amount of such lead contamination was difficult to quantify, the problem being further exacerbated by the difference in hair texture of the persons sampled. This exogenous contamination therefore detracts from the usefulness of hair as an indicator of lead exposure.     

Changes in plasma taurine concentration during a period of heroin detoxification

Taurine is one of the most abundant sulpho-amino acids in the body. Hypertaurinemia has already been reported following different stress states. A previous study demonstrated a significant increase of serum taurine concentration in heroin addicts. Therefore, we hypothesized that taurine could be a possible biomarker of recovery during detoxification from opiates. For this purpose, 30 heroin addicts who went under the 5-day heroin detoxification process were recruited for the study. Three blood samples (5 mL each) were taken from each patient in the first, third, and fifth days. They were collected in heparinized glass tubes and after centrifuging, the plasma was separated and kept in the ?20°C freezer until analysis using a previously developed HPLC method with fluorescence detection. The data were statistically analyzed using the Student t-test and ANOVA. Plasma taurine concentration in addicts was significantly more than that of the healthy controls (p < 0.0001). However, there were no changes in the plasma taurine concentration in the addicts during the 5-day study period (p > 0.05). Therefore, we can conclude that the plasma taurine concentration could not be considered as a biomarker of recovery in a 5-day detoxification period of heroin addiction.     

锑矿区人发中铋的污染状况

采用氢化物发生-原子荧光光谱法（HG-AFS）,对经过硝酸-高氯酸消解后的锡矿山矿区和贵阳市人体头发样品中重金属铋（Bi）含量进行分析。结果表明,锡矿山矿区和贵阳市人体头发中Bi的检出率分别为95.5%、22.7%,矿区居民人体头发中Bi含量显著高于作为对照的贵阳市居民人体头发中的Bi含量。锡矿山矿区男性和女性居民人发中Bi质量分数范围分别为0.0079～0.1842μg？g-1、0.0080～0.1403μg？g-1,平均值（中位数）分别为0.0480（0.0280）μg？g-1、0.0482（0.0397）μg？g-1,矿区较高的人发Bi含量主要集中在30～49岁的中年人群中。通过独立样本t检验发现,锡矿山矿区男性和女性发样中Bi含量差异不显著（p〉0.05）。研究结果说明锑矿开采和冶炼区域重金属Bi对人体健康的危害明显比非矿区严重。     

Preliminary study on health risk from mercury exposure to residents of Wujiazhan town on the Di’er Songhua river, Northeast China

Mercury concentrations in hair are typically used as a biomarker to assess exposure to mercury. A total of 108 hair samples were collected from residents (age range 5–73 years) of Wujiazhan town, northeast China, to determine total mercury concentrations. Hair mercury concentrations ranged from 0.16 to 199 mg kg^–1 with an average value of 3.41 mg kg⁻¹. The relationships between mercury concentration and gender and between hair mercury concentration and age were not significant. Overall, 16.7% of all samples were above the RfD value published by the United States Environmental Protection agency. The results indicate that there may be some been health risk from mercury exposure to the residents in the study area.     

流动注射在线萃取—火焰原子吸收光谱法测定人发中微量镉和铅

本文建立了一个流动注射在线萃取－火焰原子吸收测定人发中微量镉和铅的方法，对含Ｃｄ和Ｐｂ分别为０．０２μｇ／ｍｌ和０．２０μｇ／ｍｌ的溶液，其相对标准偏差分别为３．４％和３．８％（ｎ＝９），Ｃｄ和Ｐｂ的灵敏度分别提高２１倍和２３倍，分析速度达３６次／ｈ，Ｃｄ和Ｐｂ的回收率分别在８７．３％－９７．０％和９１．９％－１０７．３％之间，文中还详细研究了各种实验参数的选择，测定人发样的结果与文献值相符。     

人发铅、锌含量的研究

从山西省临汾市及其效区，收集了1518份健康人的头发样品（年龄从新生儿到70岁），用原子吸收光谱法测定其锌（Zn)和铅（Pb）的含量，结果表明：女性头发中锌的含量高于男性，而男性头发中铅的含量高于女性，从婴儿组（＜1岁）到青春发育组（15－19岁），发锌含量随着年龄的增长而增加，从青春发育组到老年组（61－70岁），发锌含量随着年龄的增长而降低，新生儿头发中含铅量量低，从新生儿到幼儿期91－2岁），发铅含量随着年龄的增长而增加，从幼儿期开始，随着年龄增长，发铅含量不断下降，这些结果意味着，人体中铅与锌可能是相互拮抗的，结果还表明，城市居民（除新生儿外）的发铅含量高于郊区居民的发铅含量，然而，城市和郊区居民的发锌含量未见差异。     

汞矿地区人发中甲基汞的气相色谱测定

本文采用气相色谱法测定人发中甲基汞，对人发的酸度，浸取时间，人发与酸液的比例，以及无机汞存在的影响作了测定和选择，方法的平均回收率９６．６％，精确度２．８％，方法可靠性用氢化物原子荧光法核对，结果一致，并对我国某矿区职工，儿童及产妇发样分析结果作了讨论。     

Exposure profiles of mercury in human hair at a terai belt of North India

Human hair is frequently used as a bioindicator of mercury exposure. Mercury (Hg) has for centuries been a useful metal in a variety of applications. Unfortunately, this usefulness is counterbalanced by its neurotoxicological health impact. The US Environmental Protection Agency recommends keeping the hair Hg level <1.0 µg/g. Therefore, an investigation has been performed in order to ascertain the hair Hg levels among the people living at the terai belt of North India. Hair samples were collected from 111 individuals and were placed in an identified plastic bag, stapled to prevent the shift of the hair strand. Samples were analyzed by combustion, gold amalgamation, atomic absorption spectrometry (C-GA-AAS). The mean Hg level in hair was 0.28 µg/g for the whole group ranging from 0.0012 to 1.9091 µg/g. The mean hair Hg levels were 0.16 µg/g for men and 0.12 µg/g for women, indicating that men had higher hair Hg levels than women. Total hair Hg was found to be significantly associated with age, gender and fish consumption frequency. 98 % of the total sample had hair Hg concentrations less than 1.0 µg/g, i.e, within safe dose, whereas only 2 % had Hg concentrations greater than 1.0 µg/g, thereby exceeding the safe dose.

     

Hair geochemical composition of children from Vilnius kindergartens as an indicator of environmental conditions

The research is based on analysis data of Cr, Cu, Mn, Ni, V, Zn (metals) and S in the hair of 47 girls and 63 boys from eight Vilnius kindergartens and the distribution pattern of high metal concentrations and bioavailability in snow-cover dust, also dust samples from vents of characteristic pollution sources. The kindergartens were selected according to topsoil total contamination index and dust-related indices. Significantly higher Cu, Mn, Ni and Zn concentrations in the hair of girls (means are 1.1, 1.9, 1.3, 1.2 times higher) and the differences between hair of genders according to inter-element correlation and clustering were found. Analysis of Spearman correlation coefficients between metal concentrations in hair of each gender and dust metal concentrations or metal loading rates at their residence sites revealed that for Mn, Cu and Zn, they are insignificant, while for Cr, Ni, Pb and V, they are mainly significant positive (except V in female hair). The correlation of the contents of Cr, Ni and V in dust with respective concentrations in hair was more significant for boys (p < 0.001) than for girls. Only a few cases with a significant Cr, Ni, Cu, Pb and Zn increase were revealed in hair of children attending polluted kindergartens in comparison with control. It was concluded that relationship between metal concentrations in hair and dust-related indices is more expressed for children’s residence sites than for their kindergarten sites. The gender-based grouping and site-by-site study design are recommended in the studies of reflection of environmental exposure in hair.