高效液相色谱串联质谱检测地表水中五种生物胺

采用固相萃取及高效液相色谱串联质谱技术,建立了地表水中5种生物胺（腐胺、尸胺、2-苯乙胺、酪胺、色胺）的测定方法。水样中2-苯乙胺、酪胺和色胺可直接进样测定,腐胺和尸胺经HLB固相萃取柱富集,乙腈洗脱,氮吹浓缩至1.0mL后进样液相色谱串联质谱分析,以选择离子监测（SRM）模式定量分析。在本实验条件下,加标回收率在89.4%～122%之间,相对标准偏差2.15%～11.9%（n=7）,检出限在0.05～5μg/L。     

C8-SBA-15新型介孔涂层SPME-HPLC联用测定水样中的芘

以辛基键合SBA- 15为固相微萃取(SPME)的吸附涂层,考察了吸附和解吸时间、萃取温度、搅拌速率对SPME效率的影响.该方法的线性范围为3.0-320μg/L,检出限为0.5μg/L,依据此方法测定了环境水样中芘,具有灵敏度高和精密度好的特点.     

SPE固相萃取—高效液相色谱联用测定生活废水中烷基酚

建立测定生活废水中烷基酚的SPE固相萃取—高效液相色谱联用分析方法。水样采用固相萃取柱提取富集,以甲醇和二氯甲烷洗脱,在优化的分析条件下,液相色谱法测定样品中的9种烷基酚。结果:方法的平均回收率(生活废水) 55.1%～77.4%,RSD 1.2%～20.8%。标准曲线相关系数r0.999。本方法采用固相萃取,溶剂用量少,适于生活废水中烷基酚的测定。     

在线富集-液相色谱法检测水中多环芳烃

建立了一种在线富集-液相色谱法检测水体中多环芳烃的方法,通过优化色谱条件,可不经萃取浓缩直接上机检测水样,取样体积仅为2.5 ml。除苊烯不能用荧光检测器检测外,其余15种多环芳烃的加标回收率为70.24%(苊)~117.25%(二苯并(a,h)蒽),相对标准偏差(n=5)在1.70%()~11.21%(茚并(1,2,3-c,d)芘)之间,检出限在1.51 ng/L(苯并(k)荧蒽)~44.4 ng/L(茚并(1,2,3-c,d)芘)之间,基本满足痕量分析要求。利用该方法测定实际样品中多环芳烃的浓度为0.053 ng/L(苊)~2.751 ng/L(芴)。     

C_8-SBA-15新型介孔涂层SPME-HPLC联用测定水样中的芘

以辛基键合SBA-15为固相微萃取（SPME）的吸附涂层,考察了吸附和解吸时间、萃取温度、搅拌速率对SPME效率的影响。该方法的线性范围为3.0—320μg/L,检出限为0.5μg/L,依据此方法测定了环境水样中芘,具有灵敏度高和精密度好的特点。     

介孔涂层SPME- HPLC联用测定水样中的多环芳烃

以辛基键合SBA- 15为固相微萃取(SPME)的吸附涂层,考察了吸附和解吸时间、萃取温度、搅拌速率对SPME效率的影响,该方法的线性范围分别为0.4-300μg/L、4.0-450μg/L,检出限为0.3μg/L、0.10μg/L,以此方法测定了环境水样中萘、蒽的含量.该方法具有灵敏度高和精密度好的特点.     

固相萃取-高效液相色谱法测定土壤中苯并(a)芘不确定度分析

为了建立适用于自动固相萃取结合高效液相色谱法测定土壤中苯并(a)芘含量的不确定度分析方法。采用如下方法:样品用正己烷-丙酮索式提取后,加入适量吸附剂和去离子水,经过固相萃取小柱净化、浓缩定容,再用Agilent Eclipse XDB-C18色谱柱(4.6×150mm×5μm)对苯并(a)芘含量进行分析,流动相以乙腈-水(体积比为80∶20)进行等度洗脱,采用紫外检测器检测,外标法定量。依据JJF 1135—2005《化学分析测量不确定度评定》中相关规定,考查称量、定容体积、标准曲线、仪器测量重复性和回收率等引入不确定度的主要因素,并对不确定度的各分量进行计算和合成。结果表明:当土壤样品中苯并(a)芘含量为6ng/kg时,在95%的置信区间下,其扩展不确定度为0.50ng/kg(k为2)。评定结果表明,标准曲线拟合和标准溶液配置产生的不确定度对合成不确定度的影响较大,而样品称量所引入的不确定度较小,可忽略不计。得出:该评定方法客观准确,适用于固相萃取结合高效液相色谱法测定土壤中苯并(a)芘含量的不确定度分析,对检测结果准确度的提高具有参考意义。     

搅拌棒吸附萃取气相色谱法测定地表水中多环芳烃

建立了新型的搅拌棒吸附萃取（SBSE）和热脱附系统（TDU）结合的气相色谱（GC）测定地表水中多环芳烃的方法。考察了萃取时间、搅拌条件及萃取温度对实验的影响,对7种多环芳烃（萘、荧蒽、苯并[b]荧蒽、苯并[k]荧蒽、苯并[ghi]苝、茚并[1,2,3-cd]芘和苯并[a]芘）的加标回收率为89.17%～99.38%,相对标准偏差（RSD）为1.6%～5.6%（n=3）。通过实际样品中PAHs的分析表明,该法快速、灵敏、简单,能满足痕量分析的需求。     

加速溶剂萃取-超高效液相色谱（UPLC）测定土壤中苯并（a）芘

本文优化了加速溶剂萃取-超高效液相色谱测定土壤中苯并（a）芘的方法。样品经加速溶剂提取,逐级减压浓缩,0.25um滤膜过滤净化,超高效液相色谱（UPLC）测定。结果表明,标准溶液苯并（a）芘含量在3.125～lOOug／L范围内,苯并（a）芘的线性呈良好的线性关系,相关系数为0.9999,该方法的检出限和测定下限分别为0.015μg/kg和0.060μg/kg。将该方法用于4个地区土壤样品的测定,苯并（a）芘含量在0.04～6.26ug／kg之间,空白加标回收率为75.2％～96.4％之间,各项指控指标符合检测要求。     

便携式GC-MS测定水中酚类化合物的方法研究

为实现水中酚类化合物检测的便携性,提高环境应急监测效率。建立了一种便携式固相微萃取-气相色谱/质谱联用测定水中5种酚类化合物的方法。研究了色谱柱极性、萃取柱类型、萃取温度、萃取时间、水样的pH及盐度对目标化合物分离及萃取效率和速度的影响。结果表明,使用DB-5色谱柱对目标化合物的分离效果最好;使用PDMS/DVB微萃取柱、萃取温度为70℃、萃取时间为40 min、水样的pH为3.0、NaCl浓度为0.35 g/mL时,目标物在一定浓度范围内萃取效率高、萃取速度快且线性好。方法具有较高的灵敏度,定性、定量准确,适用于水中酚类化合物的现场快速检测,能为环境应急提供重要技术支撑作用。     

回顾 总结 部署

3月26日至3月28日,备受关注的2003年度中国石油集团公司安全生产环境保护职业健康工作会议在青岛召开。 会议期间王海森主任做了题为“与时俱进,开拓创新,推进安全环境健康工作再上新水平”的报告,指出此次会议的主要任务是:总结回顾过去三年安全生产,环境保护和职业健康工作,分析形势,安排部署2003年工作,推进安全环境健康工作再上新水平。回顾三年的成绩,主要体现在:安全环保健康目标和责任制不断落实;安全环保健康规章制度逐步完善;安全环保机构得到加强和充实;健康安全环境管理体系全面推进;建设项目环境管理规范进行;安全环保科技创新…     

Sustainability,eco-efficiency,life-cycle management,and business strategy

This article outlines some of the rationale for integrating environment and sustainablility issues into core business practises and provides some guidance on how companies can begin to take a strategic view when selecting environmental management tools. Two of these tools, life cycle management and eco-efficiency, are outlined in brief.© 1999 Five Wind International. Reprinted with permission by John Wiley & Sons, Inc.     

Atrazine, isoproturon, mecoprop, 2,4-D, and bentazone adsorption onto iron oxides

Iron oxides are important components influencing the adsorption of various inorganic and organic compounds in soils and sediments. In this study the adsorption on iron oxides of nonionic and ionic pesticides was determined as a function of solution pH, ionic strength, and pesticide concentration. The investigated iron oxides included two-line ferrihydrite, goethite, and lepidocrocite. Selected pesticides comprised atrazine (6-chloro-N2-ethyl-N4-isopropyl-1,3,5-triazine-2,4-diamine), isoproturon [3-(4-isopropylphenyl)-1,1-dimethylurea)], mecoprop [(RS)-2-(4-chloro-2-methylphenoxy)propionic acid], 2,4-D (2,4-dichlorophenoxyacetic acid), and bentazone [3-isopropyl-1H-2,1,3-benzothiadiazin-4(3H)-one 2,2-dioxide]. The adsorption of the nonionic pesticides (atrazine and isoproturon) was insignificant, whereas the adsorption of the acidic pesticides (mecoprop, 2,4-D, and bentazone) was significant on all investigated iron oxides. The adsorption capacity increased with decreasing pH, with maximum adsorption reached close to the pKa values. The addition of CaCl2 in concentrations from 0.0025 to 0.01 M caused the adsorption capacity to diminish. The adsorption of bentazone was significantly lower than the adsorption of mecoprop and 2,4-D, illustrating the importance of a carboxyl group in the pesticide structure. The adsorption capacity on the iron oxides increased in the order: lepidocrocite < goethite < two-line ferrihydrite. The maximum adsorption capacities of meco-prop and 2,4-D on goethite were found to be equivalent to the site density of singly coordinated hydroxyl groups on the faces of the dominant (110) form, suggesting that singly coordinated hydroxyl groups are responsible for adsorption. Differences in adsorption capacities between iron oxides can be explained by differences in the surface site density of singly coordinated hydroxyl groups. The maximum measured adsorption capacity of mecoprop on two-line ferrihydrite was equivalent to 0.2 mol/mol Fe.     

Tillage, intercrop, and controlled drainage-subirrigation influence atrazine, metribuzin, and metolachlor loss

Atrazine (6-chloro-N2-ethyl-N4-isopropyl-1,3,5-triazine-2,4-diamine) and metolachlor [2-chloro-N-(2-ethyl-6-methylphenyl)-N-(2-methoxy-1-methylethyl)acetamide] have been found with increasing occurrence in rivers and streams. Their continued use will require changes in agricultural practices. We compared water quality from four crop-tillage treatments: (i) conventional moldboard plow (MB), (ii) MB with ryegrass (Lolium multiflorum Lam.) intercrop (IC), (iii) soil saver (SS), and (iv) SS + IC; and two drainage control treatments, drained (D) and controlled drainage-subirrigation (CDS). Atrazine (1.1 kg a.i. ha-1), metribuzin [4-amino-6-(1,1-dimethylethyl)-3-(methylthio)-1,2,4-triazine-5(4H)-one] (0.5 kg a.i. ha-1), and metolachlor (1.68 kg a.i. ha-1) were applied preemergence in a band over seeded corn (Zea mays L.) rows. Herbicide concentration and losses were monitored from 1992 to spring 1995. Annual herbicide losses ranged from < 0.3 to 2.7% of application. Crop-tillage treatment influenced herbicide loss in 1992 but not in 1993 or 1994, whereas CDS affected partitioning of losses in most years. In 1992, SS + IC reduced herbicide loss in tile drains and surface runoff by 46 to 49% compared with MB. The intercrop reduced surface runoff, which reduced herbicide transport. Controlled drainage-subirrigation increased herbicide loss in surface runoff but decreased loss through tile drainage so that total herbicide loss did not differ between drainage treatments. Desethyl atrazine [6-chloro-N-(1-methylethyl)-1,3,5-triazine-2,4-diamine] comprised 7 to 39% of the total triazine loss.     

Environmental concentrations of agricultural herbicides in Saskatchewan, Canada: bromoxynil, dicamba, diclofop, MCPA, and trifluralin

Herbicides are the most commonly used group of agricultural pesticides on the Canadian Prairies and, in 1990, more than 20000 Mg of herbicides were applied in the provinces of Alberta, Saskatchewan, and Manitoba. The present paper reports on environmental concentrations of five herbicides currently used in the prairie region. The herbicides bromoxynil [3,5-dibromo-4-hydroxy-benzonitrile], dicamba [3,6-dichloro-o-anisic acid], diclofop [(RS)-2-[4-(2,4-dichlorophenoxy)-phenoxy]propanoic acid], MCPA [(4-chloro-2-methylphenoxy)acetic acid], and trifluralin [alpha,alpha,alpha-trifluoro-2,6-dinitro-N,N-isopropyl-p-toluidine] were measured in the atmosphere, bulk atmospheric deposits, surface film, and dugout (pond) water at two sites near Regina, Saskatchewan, during 1989 and 1990. All five herbicides were detected in air and surface film and all but trifluralin were detected in the bulk atmospheric deposits and dugout water. Trifluralin was most frequently detected in air (79% of samples) whereas bromoxynil was present in maximum concentration (4.2 ng m(-3)). MCPA was present in maximum levels in bulk atmospheric (wet plus dry) deposits (2350 ng m(-2) d(-1)), surface film (390 ng m(-2)), and dugout water (330 ng L(-1)), whereas dicamba was most frequently detected in surface film (47%) and dugout water (97%). The highest quantities of the herbicides tended to be present during or immediately after the time of regional application.