反相高效液相色谱法测定污水中壬基酚聚氧乙烯醚总量

建立了固相萃取一反相液相色谱一荧光检测法分析污水中壬基酚聚氧乙烯醚总量的方法.固相萃取采用Wa-ters Oasis HLB固相萃取柱(30 μg×60 mg×3 mL),6 mL二氯甲烷/甲醇(90/10,V/V)混合溶剂洗脱,洗脱液用氮吹仪浓缩至1 mL,回收率为99.68%.采用ZORBAX Eclipse XDBC-18(4.6 mm×150 mm,5 μm)反相色谱柱,甲醇/水为流动相,流速1.0 mL/min,以每分钟增加2.5%的梯度陡度进行洗脱,流动相中甲醇比例由70%增加到100%,柱温23℃,进样量15μL.荧光检测器的激发波长230 nm,发射波长313 nm.采用外标法定量.该方法的空白加标和污水样品加标回收率均在90%以上,标准偏差小于10%,定量下限为0.97～1.90 μg/L.利用该方法分别对污水处理厂进水水样、二级处理出水水样、再生水水样进行了测定,测定结果的准确度和精密度满足痕量分析的要求.     

液相色谱/质谱联用检测刚果红及其微电解降解的研究

采用液相色谱/质谱联用(LC/MS)检测了模拟印染废水中的刚果红,并用微电解对其进行了降解研究.LC/MS检测刚果红的结果表明,在流动相为甲醇:水(体积比)=70:30、流速为0.6 mL/min、色谱柱为Zorbax XDB0-C18(150 mm× 4.6 mm,5μm)条件下,刚果红的准分子离子的质荷比(m/z)...     

单液滴微萃取—气相色谱/质谱法检测水中多环芳烃

采用单液滴微萃取-气相色谱/质谱(GC/MS)法建立了检测水中多环芳烃(PAHs)的方法,研究了萃取溶剂种类、萃取时间、搅拌速度对萃取效率的影响,确定了最佳单液滴微萃取条件,该法用于水中PAHs的检测,16种PAHs的线性范围为0.2～7.0μg/mL,相关系数≥0.9784,检出限为0.002～0.190μg/mL,相对标准偏差为7.1%～15.1%,加标回收率在81%～122%.     

固相萃取与气相色谱-质谱联用测定水中痕量多环芳烃

采用固相萃取与气相色谱-质谱联用测定水中痕量多环芳烃(PAHs)。通过正交试验,得到最佳固相萃取条件为:上样流速为5mL/min、采用二氯甲烷洗脱、洗脱剂用量为3mL、洗脱流速为2mL/min。测定结果显示,固相萃取与气相色谱—质谱联用技术对萘、菲、荧蒽3种PAHs的检出限为0.03～0.07μg/L,加标回收率为70%～100%,相对标准偏差为3.90%～9.58%。该方法精密度高、准确度好,能满足实际水样中痕量PAHs的测定要求。     

液液萃取 — 超高效液相色谱 — 三重四级杆质谱测定地表水中19种磺胺类药物残留

建立了液液萃取—超高效液相色谱—三重四级杆质谱技术,测定地表水中19种磺胺类药物。通过乙酸乙酯超声萃取水样中的磺胺类药物,并用0.1%(体积分数)甲酸水溶液-甲醇作为流动相,C18色谱柱分离,在多反应监测(MRM)模式下测定。优化了萃取剂种类和用量、超声时间、流动相的组成等条件。在优化条件下,19种磺胺类药物在0.1～40.0μg/L范围内线性良好且相关系数均大于0.999 0,方法检出限为0.02～0.80ng/L,平均回收率为73.5%～92.8%,相对标准偏差为1.2%～8.7%。该方法操作简单、灵敏度高、所需样品及有机溶剂少,适用于实际的分析检验工作。     

基于响应面分析法的水质中邻苯二甲酸酯检测方法优化

建立了水质中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DOP)的前处理及反相超高效液相色谱检测方法，通过单因素试验考察了色谱柱类型、流动相类型、流动相体积分数、流速及柱温对主峰信噪比的影响，并采用响应面分析法进行了方案优化。结果表明：氰基色谱柱优于C₁₈色谱柱；在最优色谱条件(流动相乙腈水溶液(体积分数64%)、流速0.22 mL/min、柱温28℃)下，DMP、DBP、DOP的主峰信噪比平均值分别为8 890、6 637、2 991,对应的检出限分别为0.05、0.03、0.08μg/L,均低于《水质邻苯二甲酸二甲(二丁、二辛)酯的测定液相色谱法》(HJ/T 72—2001)规定的检出限，加标回收率分别为98.4%、99.8%和98.0%,相对标准偏差为0.98%、0.52%和0.83%,具有良好的灵敏度、回收率和重复性，能更好满足地下水等水体的痕量检测要求。     

磺胺类制药废水中苯系物的快速同步检测

磺胺类制药废水是一类难降解有机废水,其中含有苯磺酰胺、苯磺酸、苯酚等苯系物,对这些物质的快速检测十分必要,针对这3种物质建立了基于高效液相色谱的快速同步检测方法。采用C18柱为分离柱,比较了乙腈/水、甲醇/水和甲醇/缓冲盐3种流动相体系的分离效果,优化了230、240、250和260 nm 4种检测波长等条件。结果表明,V甲醇∶V磷酸二氢铵溶液(0.5%,p H=3.5)=50∶50作为流动相时,基线稳定,峰形较好,3种目标物在11 min内即可实现有效分离,且浓度为5～100 mg·L~(-1)时,3种目标物峰面积与质量浓度的线性关系良好(R20.999),检出限为15.0～29.4μg·L~(-1),相对偏差为0.05%～1.56%(n=5),该方法能同时检测苯磺酸、苯酚和苯磺酰胺,具有简便、灵敏、准确等优点,可为制药废水的快速检测和磺胺类药物降解机理的分析提供便利。     

西兰花中吡蚜酮残留量的高效液相色谱检测与条件优化研究

采用正交试验,优化建立了西兰花中吡蚜酮残留量的高效液相色谱分析方法.西兰花经乙腈和二氯甲烷提取,柱层析净化后,最佳检测条件为柱温20℃、流动相为乙腈-水(体积比为85:15)、进样量10μL、流速1 mL/min.该方法对毗蚜酮的最小检出量为1.0×10-10g,最低检出质量浓度为0.005 mg/kg,西兰花平均添加回收率为87.29%～93.60%,符合农药残留检测要求.     

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。     

超声波辅助萃取—气质联用色谱法测定活性污泥中的多溴联苯醚

建立了活性污泥中多溴联苯醚(PBDEs)的分析方法。活性污泥经超声波辅助萃取,用酸性硅胶、铜粉及复合硅胶柱纯化后,采用气质联用色谱(GC/MS)对7种PBDEs单体进行测定,内标法定量。结果表明,该方法具有很好的精密性和准确性,方法检测限为17～121 pg/g,加标回收率为84.5%～109.0%,相对标准偏差(RSD)为0.5%～2.8%,回收率指示物3,3’,4,4’-四溴联苯醚(BDE-77)的回收率平均值为89.2%,RSD为0.8%,能够满足活性污泥中PBDEs的测定要求。采用所建立的方法对杭州和台州的活性污泥样品进行了测定,结果显示,台州样品中PBDEs含量高于杭州样品,但两者都低于相关文献所报道的北美及欧洲国家活性污泥中PBDEs的含量。     

大气中二（口/恶）（口/英）研究进展

二（口/恶）（口/英）是世界公认的强致癌物质,对人体健康危害极大.近年来,大气中二（口/恶）（口/英）的研究已成为各国环境化学家研究的热点.本文总结了近年来国际上有关大气中二（口/恶）（口/英）研究的进展情况,以及所取得的主要研究成果,并在此基础上指出了我国目前研究中存在的问题及以后所应开展的工作.     

Bioaccessibility of arsenic in various types of rice in an in vitro gastrointestinal fluid system

Rice can be a major contributor to dietary arsenic exposure because of the relatively high total arsenic concentration compared to other grains, especially for people whose main staple is rice. This study employed in vitro gastrointestinal fluid digestion to determine bioaccessible or gastrointestinal fluid extractable arsenic concentration in rice. Thirty-one rice samples, of which 60 % were grown in the United States, were purchased from food stores in New York City. Total arsenic concentrations in these samples ranged from 0.090 ± 0.004 to 0.85 ± 0.03 mg/kg with a mean value of 0.275 ± 0.161 mg/kg (n = 31). Rice samples with relatively high total arsenic (>0.20 mg/kg, n = 18) were treated by in vitro artificial gastrointestinal fluid digestion, and the extractable arsenic ranged from 53 % to 102 %. The bioaccessibility of arsenic in rice decreases in the general order of extra long grain, long grain, long grain parboiled, to brown rices.     

Bioaccessibility of arsenic in various types of rice in an in vitro gastrointestinal fluid system

Rice can be a major contributor to dietary arsenic exposure because of the relatively high total arsenic concentration compared to other grains, especially for people whose main staple is rice. This study employed in vitro gastrointestinal fluid digestion to determine bioaccessible or gastrointestinal fluid extractable arsenic concentration in rice. Thirty-one rice samples, of which 60 % were grown in the United States, were purchased from food stores in New York City. Total arsenic concentrations in these samples ranged from 0.090 ± 0.004 to 0.85 ± 0.03 mg/kg with a mean value of 0.275 ± 0.161 mg/kg (n = 31). Rice samples with relatively high total arsenic (>0.20 mg/kg, n = 18) were treated by in vitro artificial gastrointestinal fluid digestion, and the extractable arsenic ranged from 53 % to 102 %. The bioaccessibility of arsenic in rice decreases in the general order of extra long grain, long grain, long grain parboiled, to brown rices.     

Assessment of in situ biodegradation of monochlorobenzene in contaminated groundwater treated in a constructed wetland

The degradation of monochlorobenzene (MCB) was assessed in a constructed wetland treating MCB contaminated groundwater using a detailed geochemical characterisation, stable isotope composition analysis and in situ microcosm experiments. A correlation between ferrous iron mobilisation, decreasing MCB concentration and enrichment in carbon isotope composition was visible at increasing distance from the inflow point, indicating biodegradation of MCB in the wetland. Additionally, in situ microcosm systems loaded with 13C-labelled MCB were deployed for the first time in sediments to investigate the biotransformation of MCB. Incorporation of 13C-labelled carbon derived from the MCB into bacterial fatty acids substantiated in situ degradation of MCB. The detection of 13C-labelled benzene indicated reductive dehalogenation of MCB. This integrated approach indicated the natural attenuation of the MCB in a wetland system. Further investigations are required to document and optimise the in situ biodegradation of MCB in constructed and natural wetland systems treating contaminated groundwater.     

Bioaccumulation of decamethylcyclopentasiloxane in perch in Swedish lakes

Decamethylcyclopentasiloxane (D5), a high production volume chemical used in personal care products, enters the environment both via air and sewage treatment plant (STP) recipients. It has been found in fish, and there is concern that it may be a bioaccumulative substance. In this work D5 was analyzed in perch from six Swedish lakes that did not receive STP effluent, and in perch and sediment from six lakes that received STP effluent. In the lakes receiving the STP effluent, the D5 concentrations in sediment varied over three orders of magnitude and were correlated with the number of persons connected to the STP normalized to the surface area of the receiving body. In the lakes not receiving effluent, the D5 levels in perch were all below the LOQ, while D5 was above the LOQ in almost all perch from lakes that received effluent. The D5 concentrations in perch and sediment from the lakes receiving STP effluent were correlated. This shows that STP effluent is a much more important source of D5 to aquatic ecosystems than atmospheric deposition, and that the risk of adverse effects of D5 on aquatic life will be greatest in small recipients receiving large amounts of STP effluent. The bioaccumulation of D5 was compared to that of PCB 180 on the basis of multimedia bioaccumulation factors (mmBAFs), which describe the fraction of the contaminant present in the whole aquatic environment (i.e. water and surface sediment) that is transferred to the fish. In four of the six lakes the mmBAF of D5 was >0.3 of the mmBAF of PCB 180. Given that PCB 180 is a known highly bioaccumulative chemical, this indicates that the bioaccumulation of D5 in perch is considerable.     

Origins of Manganese in Air Participates in California

The proportions of manganese to other metals in samples of airborne fine particles taken at some sites in California have increased greatly since the beginning of 1985. Here, data are presented which indicate that the addition of manganese to leaded gasoline is largely responsible for this increase. Concentrations of manganese, silicon, titanium, iron, lead and other elements in airborne particles were measured using energy-dispersive X-ray fluorescence analysis. Coefficients of correlation among levels of manganese, iron and lead measured at twenty sites in California were calculated. Levels of manganese and iron are generally highly correlated because of the presence of large amounts of these elements in the earth’s crust. Levels of airborne manganese and lead at sites In Southern California are often highly correlated, suggesting a vehicular source of manganese. Observed manganese concentrations are apportioned into two major sources: the earth’s crust and motor vehicles. The apportionment indicates that vehicular emissions of manganese may account for a significant part of the total at urban sites in Southern California. At most other sites, the contribution from vehicles is found to be far smaller than that from the earth’s crust.     

Residues of organochlorine pesticides in fishes in Sudan

Abstract

Cotton‐producing areas of the Centrol Sudan, bordered by the Blue and the White Nile, have been subjected to repeated applications of pesticides. This region is irrigated by a series of canals, the Gezira canals, which hold large amounts of fresh water. Lake Nubia at the Sudan‐Egypt border is another important fresh water reservoir and fisheries ground. Fish from both the Gezira and Lake Nubia showed elevated concentrations of pesticides, suggesting that continued pesticides application would endanger the equatic fauna of this region and the proposed fresh water fishery.     

Involvement of glutathione in the reduction of captan-induced in vivo inhibition of monooxygenases and liver toxicity in the rat

If given orally captan is relatively nontoxic, but it can be extremely toxic after parenteral exposure. Therefore, a single i.p. dose of captan (20 mg/kg) was given to male Sprague-Dawley rats and its effect on liver microsomal mixed function oxidases and certain serum enzymes (SDH, SGPT and SGOT) was studied. The single dose of captan caused marked depression of microsomal cytochrome P-450 and the activity of benzphetamine N-demethylase and aniline hydroxylase, and moderate elevation of the serum enzymes indicative of liver damage. However, reduced glutathione (100 mg/kg, i.p.) given prior to captan, appears to decrease the liver toxicity as measured by reduced inhibition of the microsomal enzymes and elevation of serum enzymes activity. The results suggest that glutathione and other compounds containing sulfhydryl groups may protect the subjects from captan-induced liver toxicity.     

Lead concentrations in birds of prey in Britain

This paper reports on lead (Pb) concentrations in the livers of 424 individuals of 16 raptor species found dead and sent for analysis to the Institute of Terrestrial Ecology, Monkswood, from the early 1980s to the early 1990s. Elevated Pb concentrations in liver (>20 ppm dry wt), within the range associated with Pb poisoning mortality in raptors, were recorded in one peregrine (4% of species sample) and one buzzard (2% of species sample). These birds are likely to have ingested lead gunshot in the flesh of their prey. Another one each of these species had liver Pb concentrations of 15-20 ppm dry wt, reflecting unusually high absorption of Pb. No individuals of any other species had >15 ppm dry wt liver Pb, although some had 6-15 ppm. The source of Pb in these birds was unknown, but it could have resulted from high Pb concentrations in prey items, including some containing lead shot. Median liver Pb concentrations were generally very low (ranging from <0.07 to 1.61 ppm dry wt for species with sample sizes exceeding 10). In sparrowhawks, for which a large sample was available, liver Pb concentrations in all but one individual were low (<2.6 ppm dry wt). Pb concentrations in juveniles were significantly lower than in adults, and were lowest in recently fledged birds.     

饮用水中硝酸根的催化还原研究进展

由于化肥的过度使用 ,造成地下水中硝酸盐的污染日益严重。饮用水中高浓度的硝酸盐对人类健康会产生极大的威胁。本文综述了催化还原脱除水中硝酸根的研究进展和现状 ,并对其发展趋势进行了简单的论述。