首页 | 本学科首页   官方微博 | 高级检索  
相似文献
 共查询到20条相似文献,搜索用时 312 毫秒
1.
廖杰  李青松 《环境化学》2022,(5):1538-1547
大量用于预防和治疗细菌和真菌性等疾病的抗生素药物未经完全代谢后最终进入自然水体,对饮用水源水质安全构成潜在威胁.为快速测定饮用水源水体中的抗生素残留,保障饮水安全,本论文建立一种固相萃取-高效液相色谱串联质谱法测定13种抗生素的分析方法.采用OASIS? HLB小柱对水样进行固相萃取富集和净化,以甲醇和0.5%的甲酸(含5 mmol·L-1乙酸铵)水溶液为流动相,经Kinetex?C18色谱柱分离后采用三重四极杆串联质谱多反应监测模式分析.该方法检出限为0.05—1.66 ng·L-1,定量限为0.17—5.52 ng·L-1,回收率为70.2%—121.5%,相对标准偏差为1.1%—13.5%.该方法准确度高,灵敏度高,适用于饮用水源源水中痕量抗生素残留的测定.方法成功应用于厦门市饮用水源源水中抗生素残留分析,共检出7种抗生素,浓度范围为ND—32.6 ng·L-1.  相似文献   

2.
采用在线固相萃取-液相色谱-串联质谱联用(On-line SPE-LC-MS/MS)技术,建立海水循环水养殖系统中磺胺类(磺胺甲基异恶唑、磺胺噻唑、磺胺嘧啶、磺胺甲基嘧啶、磺胺二甲嘧啶)、大环内酯类(克拉霉素、脱水红霉素)、喹诺酮类(恩诺沙星、氧氟沙星、诺氟沙星)、四环素类(金霉素、四环素、土霉素)13种抗生素及孔雀石绿、隐色孔雀石绿共15种药物的同时检测方法,为循环水养殖海水中部分有机污染物的检验鉴定提供依据.采用0.1%(V/V)甲酸水溶液和0.1%(V/V)甲酸的乙腈-甲醇(1∶1,V/V)溶液为分析流动相,水样经简单酸化处理后直接进样0.9 mL进行On-line SPE-LCMS/MS检测,经在线固相萃取柱富集后,经过梯度洗脱分离,串联质谱多反应监测模式进行定性、定量分析测定.结果表明,15种目标化合物在1—100 ng·L-1范围内均具有良好的线性响应,方法检出限范围为0.02—1.00 ng·L-1,定量限范围为0.06—3.00 ng·L-1.采用该方法对山东省烟台市某水产公司2个海水循环水养殖系统的15...  相似文献   

3.
建立了同时检测水中13种典型药品及个人护理品(pharmaceuticals and personal care products,PPCPs)的固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)的分析方法.通过将HLB和WAX萃取柱串联,实现对水中污染物的固相萃取及富集净化,使用0.1%的甲酸水溶液与乙腈进行梯度洗脱,正离子多反应监测的质谱扫描模式(MRM)分析测定.13种PPCPs的检出限(LOD)为0.007—1.1 ng·L~(-1),定量限(LOQ)为0.02—3.8 ng·L~(-1),回收率为54%—97%.应用此方法调查了北京市不同类型水中PPCPs的分布情况,结果表明,该方法选择性强、操作简单、灵敏度高,可用于水样中PPCPs的可靠检测.  相似文献   

4.
建立了同时检测饮用水中6大类共12种典型药品和个人护理品(Pharmaceuticals and personal care products,PPCPs)的自动固相萃取-液相色谱-电喷雾三重四极杆串联质谱(ASPE-HPLC--ESI-MS/MS)方法.样品经ASPE(自动固相萃取)富集提取后,40℃氮吹至近干,用甲醇-水溶液(20∶80,V/V)定容至1 mL后测定.采用正离子和负离子多反应监测离子模式(MRM)定性分析,针对不同扫描模式优化流动相条件,两次进样分析.在低、中、高的3个添加水平下,12种PPCPs的方法回收率为60.8%—110%,相对标准偏差为2.0%—14.0%;检出限(LOD)为0.02—1.5 ng·L-1,定量限(LOQ)为0.06—5 ng·L-1.应用该方法调查了北京市饮用水中PPCPs污染状况,结果表明,9种PPCPs(氧氟沙星、脱水红霉素、磺胺甲恶唑、卡马西平、舒必利、普萘洛尔、萘普生、苯扎贝特和双酚A)在不同饮用水水样中被检出,最高浓度为苯扎贝特34.47 ng·L-1.该方法操作简单、灵敏度高、选择性强,符合饮用水样品中痕量污染物检测要求.  相似文献   

5.
药物和个人护理用品(Pharmaceutical and Personal Care Products,PPCPs)是在环境中长期存在并对人类乃至整个生态系统的健康造成威胁的两类化学消费品。珠江三角洲流域PPCPs的检出水平总体较高,沿海地区地下水中的PPCPs污染有待进一步探究。于2021年9月在珠海市唐家湾镇采集了16个地下水样本,使用LC-MS/MS分析技术对21种PPCPs进行检测,使用数理统计方法和相关性分析对研究区地下水中PPCPs浓度特征和污染来源进行解析,并结合地下水化学特征及统计分析对其影响因素进行探究,旨在为滨海地区地下水的PPCPs特征分析提供案例依据。研究发现,1)研究区地下水呈弱酸至弱碱性,水化学类型多属于HCO3-Ca型,沿地下水流方向受人为污染的影响越来越显著。2)研究区地下水中检测到6种PPCPs,平均质量浓度和检出率分别为:磺胺甲恶唑(5.51 ng·L-1,81%)、磺胺甲基嘧啶(1.18 ng·L-1,100%)、磺胺二甲基嘧啶(0.168 ng·L-1,25%...  相似文献   

6.
建立了在线固相萃取-高效液相色谱-串联质谱法(On-Line SPE-HPLC-MS/MS)检测地表水中8种全氟化合物(perfluorinated compounds,PFCs)的分析方法.该方法用电喷雾离子源(ESI)在选定的多反应监测(MRM)负模式下确定目标化合物并使用同位素内标法定量,测定了地表水中的PFCs. 8种PFCs的样品加标回收率在82.1%—103%之间,线性范围在0.66—500 ng·L-1之间,相关系数(R2)在0.991—0.998之间,精密度(RSD)在3.95%—6.29%之间,检出限(LOD)在0.20—2.43 ng·L-1之间,定量限(LOQ)在0.66—8.09 ng·L-1之间.方法应用于大凌河及小清河地表水的分析,分析结果与该领域其他研究的结果一致,表明该方法具有实际应用意义.  相似文献   

7.
建立了固相萃取-高效液相色谱-串联质谱法(HLB-HPLC-MS9种氟喹诺酮类(QNs)、7种大环内酯类(MCs)、3种四环素类(TCs)、2种氯霉素类(CAPs)和4种其他类(Others)共40种抗生素的分析方法.通过重点优化水样不同pH值、乙二胺四乙酸二钠(Na2EDTA)加入量、色谱条件和质谱参数等确定了最佳分析条件.水样经HLB固相萃取柱富集净化,采用Agilent Zorbax Rrhd Eclipse Plus C18 (2.1 mm×50 mm,1.8μm)色谱柱分离,正、负离子模式分别采集,正离子模式采用0.2%甲酸-2 mmol乙酸铵水溶液和甲醇-乙腈(V/V,1∶1)作流动相梯度洗脱分离38种单体;负离子模式采用纯水和甲醇-乙腈(V/V,1∶1)作流动相梯度分离2种单体,多重反应监测模式分析,内标法定量.结果显示:目标分析物线性范围在1.00—200 ng·mL~(-1)之间,相关系数r2均大于0.99,方法检出限在0.002—0.270 ng·L~(-1)之间,地表水加标回收率在61.0%—149%之间,相对标准偏差(RSD)在1.2%—32%之间.方法成功应用于贵阳市南明河12个地表水分析,共检出34种抗生素,其中大环内酯类检出浓度最高,平均浓度为257 ng·L~(-1).  相似文献   

8.
建立了食品工业废水中8种合成色素残留的固相萃取-液相色谱测定方法.水样经固相萃取柱富集,氮吹浓缩定容后直接进样.采用C18色谱柱分离,以甲醇-乙酸铵(0.01mol·L-1)溶液为流动相,进行梯度洗脱,最后利用二极管阵列检测器(DAD)进行可变波长分析,外标法定量.结果表明,8种合成色素在1.0—50mg·L-1的浓度范围内线性良好,相关系数均大于0.999,定量限为1.6—2.4μg·L-1.以实际废水样品为加标对象,分别考察了低、中、高三个浓度水平的加标回收率和精密度,平均加标回收率在82.3%—95.9%之间,精密度均小于5.45%.该方法准确可靠,灵敏度高,可用于食品工业废水中痕量色素残留的测定.  相似文献   

9.
为探究长三角地区水环境中全氟化合物(PFASs)的污染分布特征及风险水平,对长三角地区水环境中11种PFASs进行了研究.通过固相萃取结合液相色谱-三重四极杆串联质谱的方法对该地区水环境中PFASs污染水平进行分析,并运用环境风险熵值法对该地区水环境中PFASs污染进行了风险评估.结果表明PFASs在长三角地区广泛存在,Σ8PFASs浓度为8.64—736.74 ng·L-1,其中主要污染物为全氟辛酸(PFOA)、全氟己酸(PFHxA)和全氟己烷磺酸盐(PFHxS),其浓度范围分别为4.49—517 ng·L-1、0.92—688 ng·L-1和0.51—260 ng·L-1.源解析结果表明长三角大部分地区水环境中PFASs污染来源于前体化合物降解所形成的面污染源,少部分地区水环境PFASs污染来源于部分行业直接排放形成的点污染源.风险评估结果显示该地区水环境中PFASs的生态风险值和健康风险熵值均低于参考值,对生态环境和人体健康的风险水平较低.  相似文献   

10.
本文以甘肃某县为代表,对区域内冬、夏两季窖水的常规指标、17种全氟化合物和15种邻苯二甲酸酯类进行了检测,对污染来源进行了探讨,并评估了两类新污染物的健康风险.结果表明:该县窖水pH普遍偏高,夏季雨期窖水浊度显著高于冬季.新污染的检测中,共检出13种邻苯二甲酸酯类(PAEs)和14种全氟化合物(PFCs).冬季窖水中PAEs总浓度范围为2.65—3.71μg·L-1,总浓度平均值3.12μg·L-1.夏季窖水中PAEs总浓度范围为1.85—9.26μg·L-1,总浓度平均值为4.56μg·L-1.两季窖水中,邻苯二甲酸二丁酯和邻苯二甲酸二异丁酯是含量最高的成分,两种物质分别占窖水PAEs总浓度的47.8%和48.5%,窖水中PAEs没有致癌和非致癌风险.冬季窖水中PFCs的总浓度为143.93—246.47 ng·L-1,夏季为275.90—405.51 ng·L-1.检测出的PFCs包括全氟羧酸(PFCAs)和全氟磺酸(PFSAs)两大类,PFCAs占窖...  相似文献   

11.
In this paper, a method using solid-phase extraction (SPE) and gas chromatography-mass spectrometry (GC-MS) was developed to simultaneously analyze five taste and odor compounds in surface water, i.e., 2-methylisoborneol (2-MIB), 2,4,6-trichloroanisole (TCA), 2-isopropyl-3-methoxy pyrazine (IPMP), 2-isobutyl-3-methoxy pyrazine (IBMP), and trans-1,10-dimethyl-trans-9-decalol (geosmin, GSM). The mass spectrometry was operated in selective ion monitoring (SIM) mode. Three kinds of SPE columns and three eluting solvents were compared, the C18 column was chosen as optimum SPE column, and methanol was chosen as the optimum eluting solvent. It was found that the method showed good linearity in the range of 1–200 ng·L-1 and gave detection limits of 0.5–1.5 ng·L-1 for individual compounds. Good recoveries (93.5%–108%) and relative standard deviations (1.58%–7.31%) were also obtained. Additionally, concentrations of these taste and odor compounds in Jinan’s surface and drinking water were analyzed by applying this method, and the results showed that GSM and 2-MIB were the dominant taste and odor compounds in Jinan’s raw water.  相似文献   

12.
The purpose of this study was to give a worldwide overview of the concentrations of typical estrogenic endocrine disrupting chemicals (EDCs) in the effluent of sewage plants and then compare the concentra- tion distribution of the estrogenic EDCs in ten countries based on the survey data of the estrogenic EDCs research. The concentrations of three main categories (totally eight kinds) of estrogenic EDCs including steroidal estrogens (estrone (El), estradiol (E2), estriol (E3) and 17a- ethynylestradiol (EE2)), phenolic compounds (nonylphe- nol (NP) and bisphenol A (BPA)) and phthalate esters (dibutyl phthalate (DBP) and dibutyl phthalate (2- ethylhexyl) phthalate (DEHP)) in the effluents of sewage plants reported in major international journals over the past decade were collected. The statistics showed that the concentration distributions of eight kinds of EDCs were in the range of ng·L^-1 to μg·L^-1. The concentrations of steroidal estrogens mainly ranged within 50.00 ng. L-1, and the median concentrations of El, E2, E3 and EE2 were 11.00, 3.68, 4.90 and 1.00 ng·L^-1, respectively. Phenolic compounds and phthalate esters were found at pg. L-1 level (some individual values were at the high level of 40.00 μg·L^-1). The median concentrations of BPA, NP, DBP and DEHP were 0.06, 0.55, 0.07 and 0.88 μg·L^-1, respectively. The concentrations of phenolic compounds and phthalate esters in the effluents were higher than that of steroids estrogens. The analysis of the concentration in various ten countries showed that steroids estrogens, phenolic compounds and phthalate esters in sewage plant effluents were detected with high concentration in Canada, Spain and China, respectively.  相似文献   

13.
The objective of this study is to investigate the occurrence of haloacetic acids (HAAs), a group of disinfection byproducts, in swimming pool and spa water. The samples were collected from six indoor pools, six outdoor pools and three spas in Pennsylvania, the United States, and from five outdoor pools and nine indoor pools in Beijing, China. Five HAAs (HAA5), including monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, monobromoacetic acid, and dibromoacetic acid were analyzed. Total chlorine, pH and total organic carbon concentration were analyzed as well. Results indicated that the levels of HAA5 in swimming pools and spas in the United States ranged from 70 to 3980μg·L^-1, with an arithmetic average at 1440μg·L^-1 and a median level at 1150μg·L^-1. These levels are much higher than the levels reported in chlorinated drinking water and are likely due to organic matters released from swimmers' bodies. The levels of HAA5 in swimming pools in China ranged from 13 to 332μg·L^-1, with an arithmetic average at 117μg·L^-1 and a median level at 114μg·L^-1. The lower HAA levels in swimming pools in China were due to the lower chlorine residuals. Results from this study can help water professionals to better understand the formation and stability of HAAs in chlorinated water and assess risks associated with exposures to HAAs in swimming pools and spas.  相似文献   

14.
This study aimed to investigate the effects of humic acid (HA) on residual Al control in drinking water facilities that used orthophosphate addition. The results showed that adding orthophosphate was an effective method for residual Al control for the raw water without HA. When orthophosphate was added at 1.0 min before the addition of poly aluminum chloride (PACl), the concentrations of soluble aluminum (Sol-Al) and total aluminum (Tot-Al) residue were 0.08 and 0.086 mg·L-1, respectively; both were reduced by 46% compared with the control experiment. The presence of HA would notably increase the residual Al concentration. For the raw water with 5 mg·L-1 of HA, the concentrations of Sol-Al and Tot-Al increased from 0.136 and 0.174 mg·L-1 to 0.172 and 0.272 mg·L-1, respectively. For water with a HA concentration above 5 mg·L-1, orthophosphate was ineffective in the control of residual Al, though there were still parts of orthophosphate were removed in coagulation. The amounts of Al removal were positively correlated with the solids freshly formed in coagulation. Similar to the raw water without HA, the best Al control was obtained with orthophosphate salt added at 1.0 min before PACl. HA concentrations in the raw water, solution pH, and the orthophosphate dosage suitable for residual Al control by orthophosphate precipitation were also investigated.  相似文献   

15.
新型溴系阻燃剂(NBFRs, novel brominated flame retardants)作为传统溴系阻燃剂的替代品已广泛应用于电子产品、纺织品、家具等商品中,随着这些商品的生产、使用和处置,NBFRs不可避免地释放到环境中,给环境和人体带来潜在的危害.部分NBFRs可通过摄食和呼吸作用进入人体对人体产生一定危害,已被证明具有潜在的生物毒性.而NBFRs的环境污染现状研究对控制NBFRs的污染具有重要意义.近年来有不少研究者对不同环境基质中的NBFRs进行了定量测定.基于这些研究成果,本文综述了近年来环境中NBFRs的研究现状、进展,重点介绍了水体、沉积物和大气中NBFRs的含量分布.多种类型水体中NBFRs的浓度水平在ng·L-1至μg·L-1之间,浓度受地区工业生产和季节等因素影响,且不同污水处理系统对水体中NBFRs的去除效率具有一定差异;NBFRs倾向于分布在富含有机碳的介质中,沉积物中NBFRs的含量在ng·g-1至μg·g-1级别,浓度与地区工业生产、化合物性质以及总有机碳含量等因素有关;大气中的NBFRs倾向吸附于颗粒相中,在两相中的含量分别为pg·m-3和ng·g-1级别,其含量受环境因素影响较为复杂.  相似文献   

16.
以乙二胺和抗坏血酸为原料,通过一步水热法制备了水溶性的氮掺杂碳量子点(N-CQDs).研究了N-CQDs的形貌特征、光学性能和应用分析.表征结果说明,N-CQDs形态为均匀分散的球形,有明显的晶格条纹,抗光漂白性能良好,表面富有含氧官能团,具有良好的水溶性.此外发现N-CQDs还具有优良的荧光性能和荧光稳定性,量子产率可以高达12.29%.分析得出,Hg2+对N-CQDs在1.0—120μmol·L-1范围内有一定的猝灭效应,可作为Hg2+的荧光探针,检出限达230 nmol·L-1.  相似文献   

17.
• A hydrophilic resin (GCHM) was facile synthesis and characterized. • Average absolute recovery of GCHM (75.6%) performs better than Oasis® HLB. • Detection limits of method (SPE-UPLC-MS/MS) ranged between 0.03 and 0.6 ng/L. • 22 PPCPs were determined in environmental waters ranging from 0.5 to 1590 ng/L. In this study, a hydrophilic resin named GCHM was fabricated based on poly(N-vinyl pyrrolidone-co-divinylbenzene), characterized, and applied as a solid-phase extraction (SPE) material. Up to 44 pharmaceuticals and personal care products (PPCPs) belonging to 10 classes were recovered in environmental water samples. Different variables affecting extraction, such as adsorbent amount, sample pH, and loading speed, were optimized. Under optimal conditions, the average absolute recovery of 44 PPCPs was 75.6% using GCHM, indicating a better performance than the commercial Oasis® HLB. SPE with home-made hydrophilic polymeric sorbent followed by ultra-performance liquid chromatography and tandem mass spectrometry was validated, and the method achieved good linearity (r2>0.991, for all analytes). In addition, the method detection limits of target compounds ranged from 0.03 to 0.6 ng/L. The developed method was applied to determine PPCPs in 10 environmental water samples taken from the Yangtze River, Huaihe River, and Taihu Lake, 1 groundwater sample from Changzhou in Jiangsu Province, 1 wastewater sample from Xiamen and 2 seawater samples from the Jiulong River in Fujian Province, China. In these samples, 22 compounds were determined at levels ranging from 0.5 to 1590 ng/L.  相似文献   

18.
High-affinity and specific monoclonal antibodies against cadmium-ethylene diamine tetraacetic acid (EDTA) complex have been produced using the hybridoma technique. A hapten was synthesized and characterized by Fourier Transform Infrared Spectroscopy (FT-IR) and UV-Vis. Competitive enzyme-linked immunosorbent assay (ELISA) for quantitative detection of cadmium in aqueous sample was developed. The monoclonal antibody with high level of binding affinity for Cd-IEDTA-BSA and high specificity for soluble Cd-EDTA complex showed less than 0.99% cross-reactivity with other 11 metals. The limit of detection was 0.10 μg·L-1, and the effective linear range was 10-1–103 μg·L-1. The intra- and inter-assay coefficient variations were 1.5%–6.3% and 3.2%–7.4%, respectively. The spike recovery in different water samples were between 98.5% and 110.3%. The detection limit of this assay was well below the allowable concentration of cadmium (3 μg·L-1), and the working range was wider than that of other methods which showed the range of 2.19–86.38 and 0–103 μg·L-1. The competitive ELISA established in this paper was sensitive and accurate in the screening of cadmium in aqueous samples. The results will lay a solid foundation for construction of an immunoassay kit for cadmium.  相似文献   

19.
The efficient removal of phosphorous from water is an important but challenging task. In this study, we validated the applicability of a new commercially available nanocomposite adsorbent, i.e., a polymer-based hydrated ferric oxide nanocomposite (HFO-201), for the further removal of phosphorous from the bioeffluent discharged from a municipal wastewater treatment plant, and the operating parameters such as the flow rate, temperature and composition of the regenerants were optimized. Laboratory-scale results indicate that phosphorous in real bioeffluent can be effectively removed from 0.92 mg·L-1 to<0.5 mg·L-1 (or even<0.1 mg·L-1 as desired) by the new adsorbent at a flow rate of 50 bed volume (BV) per hour and treatable volume of 3500–4000 BV per run. Phosphorous removal is independent of the ambient temperature in the range of 15°C–40°C. Moreover, the exhausted HFO-201 can be regenerated by a 2% NaOH+ 5% NaCl binary solution for repeated use without significant capacity loss. A scaled-up study further indicated that even though the initial total phosphorus (TP) was as high as 2 mg·L-1, it could be reduced to<0.5 mg·L-1, with a working capacity of 4.4–4.8 g·L-1 HFO-201. In general, HFO-201 adsorption is a choice method for the efficient removal of phosphate from biotreated waste effluent.  相似文献   

20.
The reduction of hexavalent chromium by scrap iron was investigated in continuous long-term fixed bed system. The effects of pH, empty bed contact time (EBCT), and initial Cr(VI) concentration on Cr(VI) reduction were studied. The results showed that the pH, EBCT, and initial Cr(VI) concentration significantly affected the reduction capacity of scrap iron. The reduction capacity of scrap iron were 4.56, 1.51, and 0.57 mg Cr(VI)·g-1 Fe0 at pH 3, 5, and 7 (initial Cr(VI) concentration 4 mg·L-1, EBCT 2 min, and temperature 25°C), 0.51, 1.51, and 2.85 mg Cr(VI)·g-1 Fe0 at EBCTs of 0.5, 2.0, and 6.0 min (initial Cr(VI) concentration 4 mg·L-1, pH 5, and temperature 25°C), and 2.99, 1.51, and 1.01 mg Cr(VI)·g-1 Fe0 at influent concentrations of 1, 4, and 8 mg·L-1 (EBCT 2 min, pH 5, and temperature 25°C), respectively. Fe(total) concentration in the column effluent continuously decreased in time, due to a decrease in time of the iron corrosion rate. The fixed bed reactor can be readily used for the treatment of drinking water containing low amounts of Cr(VI) ions, although the hardness and humic acid in water may shorten the lifetime of the reactor, the reduction capacity of scrap iron still achieved 1.98 mg Cr6+·g-1 Fe. Scanning electron microscope equipped with energy dispersion spectrometer and X-ray diffraction were conducted to examine the surface species of the scrap iron before and after its use. In addition to iron oxides and hydroxide species, iron-chromium complex was also observed on the reacted scrap iron.  相似文献   

设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号