用SPME测定珠江河口水体中的PCBs

报道了利用SPME技术结合电子捕获检测气相色谱 (ECD)测定珠江入海河口水体中PCBs有机污染物的含量 ,并讨论了SPME装置萃取PCBs的主要影响因素。结果表明 :在选取一定的萃取纤维头 (10 0 μmPDMS)后 ,影响萃取效果的主要因素是萃取时间的长短 ,其次为萃取的温度和pH值。在各个影响因素及不同水平处理中 ,以萃取时间 30min、萃取温度 35℃、pH值 7.2、搅拌速度 10 0 0r/min为最理想。在该种条件下测定了珠江入海四大口门虎门、横门、蕉门和斗门河口水体中PCBs含量分别为 2 .70 1、0 .999、2 .82 8和 1.16 1ng/L。     

新型循环冷凝固相微萃取方法的研究

首次提出一种新型循环冷凝萃取(CC-SPME)方法,并以乙硫醚为研究对象进行了分析检测。实验优选条件得出CC-SPME法的萃取时间,溶液加热温度和解吸时间分别为25min,75℃,4min。该方法的重现性,检测限以及回收率分别为7.54%,0.010mg/L,97%。实验表明,此方法的线性很好,而且与传统的浸入萃取法和顶空萃取法相比,具有更高的灵敏度。故而CC-SPME法是一种简单且灵敏的分析检测方法,值得做进一步探讨。     

Determination of 27 pharmaceuticals and personal care products (PPCPs) in water: The benefit of isotope dilution

• Isotope dilution method was developed for the determination of 27 PPCPs in water. • The established method was successfully applied to different types of water samples. • The correction effect of corresponding 27 ILSs over 70 d was investigated. • Benefit of isotopic dilution method was illustrated for three examples. Pharmaceuticals and personal care products (PPCPs) are a unique group of emerging and non-persistent contaminants. In this study, 27 PPCPs in various water samples were extracted by solid phase extraction (SPE), and determined by isotope dilution method using liquid chromatography coupled to tandem triple quadruple mass spectrometer (LC-MS/MS). A total of 27 isotopically labeled standards (ILSs) were applied to correct the concentration of PPCPs in spiked ultrapure water, drinking water, river, effluent and influent sewage. The corrected recoveries were 73%–122% with the relative standard deviation (RSD)<16%, except for acetaminophen. The matrix effect for all kinds of water samples was<22% and the method quantitation limits (MQLs) were 0.45–8.6 ng/L. The developed method was successfully applied on environmental water samples. The SPE extracts of spiked ultrapure water, drinking water, river and wastewater effluent were stored for 70 days, and the ILSs-corrected recoveries of 27 PPCPs were obtained to evaluate the correction ability of ILSs in the presence of variety interferences. The recoveries of 27 PPCPs over 70 days were within the scope of 72%–140% with the recovery variation<37% in all cases. The isotope dilution method seems to be of benefit when the extract has to be stored for long time before the instrument analysis.     

热解析-固相微萃取-气相色谱法测定空气样品中挥发性有机化合物

建立了热解析-固相微萃取-气相色谱法测定空气样品中挥发性有机化合物的分析方法,并对色谱分离条件、玻璃针筒保存样品的稳定性、固相微萃取萃取纤维、萃取时间、色谱进样时间等条件进行了优化,9种挥发性有机化合物的峰面积与其质量浓度在所测范围内有较好的线性关系,相对标准偏差＜8.8%,检出限为0.05～0.75 μg/100 mL,满足实际空气样品测定需要。     

Determination of antibiotics in sewage from hospitals, nursery and slaughter house, wastewater treatment plant and source water in Chongqing region of Three Gorge Reservoir in China

Sewage samples from 4 hospitals, 1 nursery, 1 slaughter house, 1 wastewater treatment plant and 5 source water samples of Chongqing region of Three Gorge Reservoir were analyzed for macrolide, lincosamide, trimethoprim, fluorouinolone, sulfonamide and tetracycline antibiotics by online solid-phase extraction and liquid chromatography-tandem mass spectrometry. Results showed that the concentration of ofloxacin (OFX) in hospital was the highest among all water environments ranged from 1.660 μg/L to 4.240 μg/L and norfloxacin (NOR, 0.136-1.620 μg/L), ciproflaxacin (CIP, ranged from 0.011 μg/L to 0.136 μg/L), trimethoprim (TMP, 0.061-0.174 μg/L) were commonly detected. Removal range of antibiotics in the wastewater treatment plant was 18-100% and the removal ratio of tylosin, oxytetracycline and tetracycline were 100%. Relatively higher removal efficiencies were observed for tylosin (TYL), oxytetracycline (OXY) and tetracycline (TET)(100%), while lower removal efficiencies were observed for Trimethoprim (TMP, 1%), Epi-iso-chlorotetracycline (EICIC, 18%) and Erythromycin-H₂O (ERY-H₂O, 24%). Antibiotics were removed more efficiently in primary treatment compared with those in secondary treatment.     

Detection of DDT and its metabolites in two estuaries of South China using a SPME-based device: First report of p,p′-DDMU in water column

A solid-phase microextration-based sampling method was employed to determine the concentrations of 1,1,1-trichloro-2,2-bis(p-chlorophenyl)ethane (DDT) and its metabolites, 1,1-dichloro-2,2-bis(p-chlorophenyl)ethane (DDD), 1,1-dichloro-2,2-bis(p-chlorophenyl)ethene (DDE) and 1-chloro-2,2-bis(p-chlorophenyl)ethene (DDMU), in two estuarine bays, Daya Bay and Hailing Bay, of South China. Six DDT components including p,p′-DDT, o,p′-DDD, p,p′-DDD, o,p′-DDE, p,p′-DDE, and p,p′-DDMU were detected in Hailing Bay, while only p,p′-DDD was found in Daya Bay. p,p′-DDD was the most abundant DDT component in both bays, sharply different from the previous finding in the water column of the Palos Verdes Shelf, California, USA that p,p′-DDE was prevalent. In addition, the occurrence of p,p′-DDMU (with a range of 0.047-0.21 ng/L in Hailing Bay) has not been reported around the globe, and its presence in our study region appeared to stem from dehydrochlorination of p,p′-DDD, favored under aerobic conditions, but further investigations are clearly needed to confirm the mechanism for generation of DDMU in estuarine environments.     

盐析分相微萃取—高效液相色谱法测定水中含氯除草剂

采用盐析分相微萃取—高效液相色谱法同时测定水中3种含氯除草剂,建立并优化了反相离子对液相色谱条件,考察了萃取剂种类、盐析剂的种类和加入量及试样pH对萃取效果的影响。对氯苯氧乙酸、2,4-二氯苯氧乙酸和2,4-滴丁酯的质量浓度在0.1~100.0mg/L内与色谱峰面积呈良好的线性关系,相关系数不低于0.9992。平均回收率分别为96.29%、79.16%和70.21%,相对标准偏差小于5.3%。该方法操作简便、绿色环保,适合于水中含氯除草剂的测定。     

固相微萃取-气相色谱/质谱联用法测定饮用水中苯类化合物

用固相微苹取(ＳＰＭＥ)－气相色谱/质谱联用法测定饮用水中苯类化合物,以１００μｍ ＰＤＭＳ(聚二甲基硅氧烷)萃取针提取、浓缩、分离与测定九种目标化合物．萃取时间经优化选定为８ｍｉｎ,而热解析时间设定为２ｍｉｎ． 本方法的相对标准偏差小于５%,线性范围宽(２０ｎｇ·ｍｌ－１－１００００ｎｇ·ｍｌ－１),多数化合物的检测限低于５μｇ·ｌ－１．饮用水样品检测显示,样品加标回收率范围在８４%至１１０%内．     

固相微萃取-气相色谱法测定生活污水中壬基酚

采用固相微萃取-气相色谱法测定生活污水中的壬基酚,优化了萃取纤维涂层材料、萃取时间与温度、解析时间与温度、盐度、pH值、搅拌速度等试验参数。方法在0.001mg／L-1.00mg／L范围内线性良好,检出限为0.0006mg／L,标准溶液平行测定的RSD为7.6％,生活污水加标回收率为42.7％-74.0％。     

固相萃取- GC/MS法测定水中邻苯二甲酸酯类

采用固相萃取-GC／MS法测定水中6种邻苯二甲酸酯类有机污染物,比较了不同固相萃取柱对萃取效果的影响,优化了水样pH值、水样流量、穿透体积、洗脱溶剂、洗脱剂体积、洗脱流量等萃取条件。方法在0．050μg/L-800μg/L范围内线性良好,检出限为0．008μg/L～0．03μg／L,标准溶液测定的RSD≤10．5％,实际水样加标回收率为80．0％-100％。