水中微量磺胺甲恶唑的现场快速前处理方法
Rapid in-situ sample pretreatment method for the analysis of trace sulfamethoxazole in water
-
摘要: 本文制备了磺胺甲恶唑分子印迹聚合物,通过静态吸附实验及红外光谱等手段研究其性能,并以该聚合物为核心材料自制液体样品快速前处理装置,建立且优化出一种水溶液中微量磺胺甲恶唑的简单、经济的现场批量前处理方法.通过加标回收实验验证了该方法的可行性,并进行了实际样品的现场前处理与测定.结果表明,所制备的印迹聚合物(MIP)具有良好的亲和性和特异选择性;在0.50—1000.00 μg·L-1范围内,所建立方法的水样加标回收率为72.0%—100.3%,相对标准偏差为2.2%—5.1%(n=6),方法的检测限为0.01 μg·L-1.本实验所采集的5种实际样品(红湖水样、水上乐园水样、鱼塘水样、牛尿和猪尿)中均检出磺胺甲恶唑,其浓度分别为0.76、1.23、1.94、202.0、435.3 μg·L-1.Abstract: Molecularly imprinted polymers for sulfamethoxazole were prepared as a critical material to establish a rapid in-situ pretreatment method for measuring trace sulfamethoxazole in water. Properties of the molecularly imprinted polymers for sulfamethoxazole were studied by means of the infrared spectroscopy and static adsorption experiment. A simple and economic pretreatment device was assembled in this experiment. The feasibility of the method was verified by combining it with high performance liquid chromatography (HPLC) in the spiked recovery experiment. Real samples were collected and treated with this method, and results showed that molecularly imprinted polymer (MIP) had good affinity and specific selectivity. As the concentration of sulfamethoxazole in water ranged from 0.50 μg·L-1 to 1000.00 μg·L-1, the spiked recoveries of sulfamethoxazole ranged from 72.0% to 100.3%, relative standard deviation ranged from 2.2% to 5.1%(n=6), the detection limit of this method was 0.01μg·L-1. Three surface water samples and two urine samples were collected and pretreated in-situ with the method and then analyzed with HPLC in the lab. Results indicated that sulfamethoxazole concentrations in surface water samples, aquaculture water and urine solution were 0.76, 1.23, 1.94, 202.0, 435.3 μg·L-1, respectively. The method could be used for rapid in-situ pretreatment of field samples, which could be employed for automatic monitoring.
-
Key words:
- sample pretreatment /
- method /
- solution /
- sulfamethoxazole /
- molecularly imprinted polymer
-
[1] BRUCE J R, PAUL K S L, Michael M. Emerging chemicals of concern: Pharmaceuticals and personal care products (PPCPs) in Asia, with particular reference to Southern China[J]. Marine Pollution Bulletin, 2005, 50: 913-920. [2] 李俊锁,邱月明,王超,等. 兽药残留分析[M]. 上海: 上海科学技术出版社, 2002: 228-264. LI J S, QIU Y M, WANG C, et al. Veterinary drug residue analysis [M]. Shanghai: Shanghai Science and Technological Press, 2002: 228 -264(in Chinese).
[3] HALLING-SORENSEN B, NIELSN S N, LNZKY P F, et al. Occurrence, fate and effect of pharmaceutical substances in the environment: A review[J]. Chemosphere, 1998, 36 (2): 357-39. [4] HARTMANN A, ALDER A C, KOLLER T, et al. Identification of fluoroquinolone antibiotics as the main source of human genotoxicity in native hospital wastewater[J]. Environmental Toxicology and Chemistry, 1998, 17: 377-382. [5] DAUGHTON C G, TERNES T A. Pharmaceuticals and personal care products in the environment: Agents of subtle change[J]. Environmental Health Perspectives. 1999, 107: 907-938. [6] SUNG C K, KENNETH C. Quantification of human and veterinary antibiotics in water and sediment using SPE/LC/MS/MS[J]. Analytical and Bioanalytical Chemistry, 2007, 387: 1301-1315. [7] 徐浩, 肖湘波, 唐文浩 等.海口城区地表水环境中抗生素含量特征研究[J]. 环境科学与技术, 2013, 36(9): 60-65. XU H, XIAO X B, TANG W H et al. Concentration characteristics of antibiotics in urban aquatic environment of Haikou[J]. Environmental Science & Technology, 2013, 36(9): 60-65(in Chinese).
[8] TONG L, LI P, WANG Y X, et al. Analysis of veterinary antibiotic residues in swine wastewater and environmental water samples using optimized SPE-LC/MS/MS[J]. Chemosphere, 2009, 74: 1090-1097. [9] 张金, 宗栋良, 常爱敏, 等. 水环境中典型抗生素 SPE-UPLC-MS/MS检测方法的建立[J]. 环境化学,2015,34(8): 1446-1452. ZHANG J, ZONG D L, CHANG A M, et al. Determination of common antibiotics in aquatic environment by solid-phase extraction and ultra pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)[J]. Environmental Chemistry, 2015, 34(8): 1446-1452(in Chinese).
[10] BEN W W, QIANG Z M, ADAMS C, et al. Simultaneous determination of sulfonamides, tetracyclines and tiamulin in swine wastewater by solid-phase extraction and liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2008, 1202: 173-180. [11] 孙奉翠. 土壤中四类典型抗生素的同时测定及其方法优化[D]. 山东: 山东大学硕士学位论文, 2013. SUN F C. Simultaneous determination of four kinds of typical antibiotics in soil and method optimization[D]. Shandong, Shandong University, 2013(in Chinese). [12] 陈海燕. 土壤中三种磺胺类抗生素HPLC检测方法及污染分布研究[D]. 安徽: 安徽农业大学硕士学位论文, 2011. CHEN H Y. Study on the HPLC detection method and distribution of three sulfonamides antibiotics in soil[D]. Anhui: Anhui Agricultural University, 2011(in Chinese). [13] VALERO-NAVARRO A, GOMEZ-ROMERO M. Synthesis of caffeic acid molecularly imprinted polymer microspheres and high-performance liquid chromatography evaluation of their sorption properties[J]. Journal of Chromatography A, 2011, 1218(41): 7289-7296. [14] LI Y, FU Q, LIU M, et al. Separation and enrichment of trace ractopamine in biological samples by uniformly-sized molecularly imprinted polymers[J]. Journal of Pharmacology Analysis, 2012, 6(2): 395- 402. [15] JI S L, ZHANG F F, LUO X, et al. Synthesis of molecularly imprinted polymer sorbents and application for the determination of aminoglycosides antibiotics in honey[J]. Journal of Chromatography A, 2013, 1313: 1113-118. [16] 杜碧柏, 许杨, 黄云红, 等. 分子印迹固相萃取-高效液相色谱法测定饲料中磺胺类药物[J]. 分析化学, 2012, 40(12): 1871-1876. DU B B, XU Y, HUANG Y H, et al. Determination of sulfonamides in feeds by high performance liquid chromatography with molecularly imprinted solid phase extraction[J]. Chinese Journal of Analytical Chemistry, 2012, 40(12): 1871-1876(in Chinese).
计量
- 文章访问数: 672
- HTML全文浏览数: 580
- PDF下载数: 441
- 施引文献: 0