高效液相色谱-串联质谱法同时检测地表水中13种药物及个人护理品

采用高效液相色谱-串联质谱(HPLC-MS/MS)检测,建立了地表水中13种药物及个人护理品的测定方法。水样用盐酸与氢氧化钠溶液调p H值至7.0左右,过固相萃取小柱进行富集,用14 m L甲醇洗脱。以C18柱为分离柱,0.01%甲酸的甲醇-0.01%甲酸水溶液为流动相,目标物在10 min内分离,在0.50~250μg/L范围内,13种化合物峰面积与内标物质峰面积之比与质量浓度的线性关系良好(0.99),检出限在0.05~0.5 ng/L范围内。基质加标实验结果表明,13种化合物在水中的回收率分别在56.2%~123.2%之间(加标水平5 ng/m L)和58.0%~107.8%(加标水平50 ng/m L),相对标准偏差在1.60%~19.9%(n=6)之间。应用该方法测定了从2条纳污河流采集的10份水样,结果表明,除美托诺尔和普洛萘尔未被检出外,其余11药物的检出频率在30%~100%之间。在13种目标物质中,咖啡因的检测浓度最高达287.5ng/L,舒必利次之,为277.5 ng/L。本方法快速、准确,适用于地表水中PPCPs类的快速测定。     

A method for determining the analytical form of a radionuclide depth distribution using multiple gamma spectrometry measurements

When characterizing environmental radioactivity, whether in the soil or within concrete building structures undergoing remediation or decommissioning, it is highly desirable to know the radionuclide depth distribution. This is typically modeled using continuous analytical expressions, whose forms are believed to best represent the true source distributions. In situ gamma ray spectroscopic measurements are combined with these models to fully describe the source. Currently, the choice of analytical expressions is based upon prior experimental core sampling results at similar locations, any known site history, or radionuclide transport models. This paper presents a method, employing multiple in situ measurements at a single site, for determining the analytical form that best represents the true depth distribution present. The measurements can be made using a variety of geometries, each of which has a different sensitivity variation with source spatial distribution. Using non-linear least squares numerical optimization methods, the results can be fit to a collection of analytical models and the parameters of each model determined. The analytical expression that results in the fit with the lowest residual is selected as the most accurate representation. A cursory examination is made of the effects of measurement errors on the method.     

超声波提取-恒波长同步荧光法测定淡水藻中叶绿素a的含量

针对绿藻,采用超声波提取,以荧光激发-发射波长差216nm,建立了同步荧光法测定绿藻叶绿素a含量的新方法,其线性范围为0.02～1.25 mg/L,检出限为1.6ug/L,加标回收率在97.0%～104%之间。与分光光度法测定叶绿素a的对比试验结果表明,两者无显著性差异,但该方法具有快速、灵敏,其他常见色素不干扰测定的优点,能够满足供水中绿藻叶绿素a含量快速检测的需要。     

固相萃取-超高效液相色谱-串联质谱测定水中痕量苯甲地那铵

苯甲地那铵是一种广泛使用的苦味剂,近年来被发现在欧洲水体中普遍存在。建立灵敏可靠的环境样品前处理分析方法对评价其环境行为具有重要意义。通过优化关键前处理过程参数,建立了水中苯甲地那铵的固相萃取-超高效液相色谱串联质谱分析方法,系统考察了该方法的准确度、精密度、基质效应、检出限以及线性范围。研究表明：当调节水样pH至8以上,采用混合型阳离子交换小柱(200 mg, 3 mL)富集水样,采用含体积分数2%甲酸的甲醇溶液洗脱时,该方法可获得最佳回收率;纯水和环境水样中加标回收率分别为97%～105%和89%～119%,相对标准偏差小于7%;基质效应均在24%以内;方法检出限为0.07 ng/L,线性范围为0.01～50μg/L。该方法可用于环境水体中苯甲地那铵的痕量检测。     

加速溶剂萃取-固相萃取-高效液相色谱/三重四级杆质谱法测定土壤中6种喹诺酮类抗生素残留

为测定污染土壤中的6种低残留喹诺酮类抗生素(氧氟沙星、培氟沙星、恩诺沙星、环丙沙星、诺氟沙星、恶喹酸),全面优化了一种联合加速溶剂萃取(ASE)、固相萃取(SPE)和高效液相色谱/三重四级杆质谱(HPLC/MSMS)3种检测技术的分析方法.样品采用甲醇和0.1 mol/L EDTA-McIlvaine缓冲液(1∶1)进...     

Comparison of Three Extraction Methods for 17 β-Estradiol in Sand,Bentonite, and Organic-Rich Silt Loam

Extraction is an important procedure for samples that contain soil because other compounds in soil may affect analysis of estrogens. This study was conducted to evaluate three different extraction methods for 17β-estradiol in soil. Sand, bentonite, and organic-rich silt loam were spiked with 1 mg kg^{? 1} of 17β-estradiol as a model compound of estrogens. 17β-estradiol and its metabolites, estrone and estriol, were extracted using (i) a modified Bligh and Dyer extraction, (ii) a pressurized fluid extraction, and (iii) a diethyl ether extraction, and measured by liquid chromatography tandem mass spectrometry. There were significant differences in the extraction efficiency for 17β-estradiol among the extraction methods and the soils: the efficiencies ranged from 10% to 97%. Overall, the diethyl ether extraction method had the largest efficiency of 17β-estradiol with 45% and 57% for bentonite and silt loam, respectively. Transformation of 17β-estradiol to estrone and estriol in the different extraction methods was less than 3.6% during the extraction procedures. This study underlined the importance of sample preparation for estrogen analysis in soil samples.     

DECISION-MAKING PROCESS ON THE DANUBE AND THE PLATTE1

ABSTRACT: Two case studies highlighting the institutional arrangements and decision-making processes used to attempt to allocate water on large scale river systems in two countries are presented. In both cases the implementation of river plans has been blocked by conflicts between those who wish to use water for irrigation, hydropower, or municipal purposes and those who wish to maintain instream flows for fish and wildlife. To date conflict has blocked the implementation of a large hydropower scheme on the Danube River, downstream from Vienna, Austria, and the construction of municipal and agricultural projects, as well as the relicensing of an existing hydropower facility on the Platte River in Nebraska. Analysis of the decision-making processes and institutional settings of both cases led to the identification of problem areas and development of recommendations that would support the achievement of compromise solutions for management.     

原子吸收石墨炉技术测定水中痕量阴离子洗涤剂

本文研究了用乙二胺铜(Ⅱ)—氯仿作为络合—萃取体系,石墨炉原子吸收技术间接测定水中痕量阴离子洗涤剂的一种方法。其检出限为2.0ug/1,加标回收率为89.6%～104.5%。具有选择性好、灵敏度高、快速简便等特点。同时还研究了水样的酸度和共存离子对测定的影响。对于用原子吸收进行有机分析具有一定的实际意义。     

The Colorado,USA, Joint Review Process: an initial evaluation of its success as a permit reform by key participants

Colorado, USA, developed the Joint Review Process (CJRP) in 1978 to coordinate the application and review of permits required for major development projects. Since then, the state has used the process on over 20 projects. This study examined whether the CJRP has achieved its primary goals—enhanced coordination of agencies, enhanced public participation, and strengthened communication between agencies and project sponsors— and several related secondary goals. The success of the process was measured through a survey of 54 key people who had been directly involved with the process. Those surveyed included federal and state agency staff, local agency managers, corporate officers, private consultants, and environmental leaders. All groups, with one exception, agreed that the process achieved its primary goals and that it should be retained. Environmental leaders were neutral about whether the process enhanced public participation and about retaining the process. The report concludes with a review of recommended improvements to and applications of the CJRP.     

AAS与ICP－AES间接测定天然水中硫酸盐

本文以与过量形成ＢａＳＯ＿４沉淀反应为基础，较详细地讨论了反应条件、从而拟定了用ＡＡＳ和ＩＣＰ－ＡＥＳ间接测定天然水中的方法、确定了方法的精密度，ＡＡＳ法的ＲＳＤ％为１．５，ＩＣＰ－ＡＥＳ法为３．２．两种方法对比分析的结果接近，误差为１．０％（相对）。用于天然水中的测定，获得满意的结果。