水环境抗生素分析及全国沿岸陆源排海浓度分布研究
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摘要
抗生素不但在世界范围内用于人类和动物治疗感染疾病,而且还作为畜牧业的生长促进剂使用。人畜服用的药物很大部分在生物体内没有经过代谢,最终进入水环境中。由于抗生素可能对微生物群落产生耐药性的特殊性,他们在环境中存在的浓度及其环境行为越来越受到重视。本研究特别针对人和动物治疗疾病较为常用的磺胺类抗生素和氯霉素给予关注。
应用固相萃取(SPE)及LC-MS/MS技术,建立了水中痕量磺胺类抗生素的分析方法,优化了固相萃取、液相色谱.串联质谱等相关条件。水样经H LB固相萃取柱富集净化,采用电喷雾离子源,在正离子检测模式下,以多反应监测模式(MRM)对待测物进行定性和定量分析。除磺胺噻唑(STZ)为3 ng/L外,其余检出限为1 ng/L。加标水样的回收率在22.3%～87.0%之间,采用外标法定量。该方法灵敏度高、选择性好、准确度高,适合实际水样中痕量磺胺类药物的检测。
应用液液萃取高效液相色谱-串联质谱法测定水中的氯霉素残留,流动相为甲醇:水(80:20)。采用负电喷雾离子源,在多反应性监测模式下采集信号,定性离子对为321/121、321/152、321/176,定量离子对为321/152。本方法的线性范围是0.1μg/L～100μg/L,其相关系数为0.9993,方法检出限为10 ng/L,回收率在81.7%～121.0%之间。还建立了超声波辅助萃取,高效液相色谱测定沉积物中的氯霉素残留的方法。
2006年开展中国沿岸陆源抗生素排海浓度分布的调查。排污口水域已经受到磺胺类化合物的药物污染,低于国外地表水的污染水平。但是,随着其大量生产及应用,污染问题也变得越来越严重。城市生活污水排放是入海水域磺胺类污染物的主要来源。在所有54个排污口水样品中,未检出氯霉素残留。对大连近岸海域养殖环境进行调查,在水样品中发现氯霉素残留。
Antibiotics are not only administered worldwide in human and animal medicine for the treatment of infections but are an integral part of modern animal production. After consumption, a great part of antibiotic pharmaceuticals mainly enter the environment unmetabolited and can eventually reach the aquatic environment. Their environmental occurrence and fate is of particular interest, due to the potential spread and maintenance of antibacterial resistance. The research focuses on the sulfonamides and chloramphenicol, which are used frequently as human and animal medicines.
This research developed a rapid method for the determination of 14 kinds of sulfonamides (SAs) in wastewater using solid-phase extraction (SPE), and liquid chromatography tandem mass spectrometry (LC-MS/MS) with positive electrospray ionization (ESI(+)) and multiple reaction monitoring (MRM) mode. The SPE was performed on an Oasis HLB cartridge. Chromatographic separation on a C18 column was achieved using a binary eluent containing methanol and water with 0.2% formic acid. Typical recoveries of the analytes ranged from 22.3% to 87.0% at a fortification level of 100 ng/L. The limits of detection (LOD) in wastewater except sulfathiazole (3 ng/L) could be detected and quantified at levels as low as 1 ng/L.
Chloramphenicol in water was extracted liquid-liquid extraction and determined by HPLC-MS/MS, using methanol-water (80:20) as the mobile phase. The spectral acquisition was done in the negative electron spray ionization utilizing multiple reaction monitoring of three parent- daughter ion pairs: m/z 321/121, 321/152 and 321/176. The ion pair of m/z 321/152 was used for quantitation. Linear plots were obtained between 0.1μg/L and 100μg/L, with linear correlation coefficient of 0.9993. The limit of detection was 10 ng/L. Ultrasonic assistance extraction followed by HPLC analysis was applied for the determination of the concentration in the sediment samples.
In 2006, an antibiotic monitoring campaign was carried out, which focused on the distribution in the coastal zone of China by the discharge of land-based wastewater. The result shows the water occurred the sulfonamide antibiotics' residue. But they are lower than the water pollution level in the developed countries. However, with its large-scale production and application, the problem of pollution is becoming more and more serious. The municipal wastewater discharge is the most important source of sulfonamides in these sites. All 54 water samples have not been detected chloramphenicol residues. For the investigation in aquaculture environment, water samples were found chloramphenicol residues.
应用固相萃取(SPE)及LC-MS/MS技术,建立了水中痕量磺胺类抗生素的分析方法,优化了固相萃取、液相色谱.串联质谱等相关条件。水样经H LB固相萃取柱富集净化,采用电喷雾离子源,在正离子检测模式下,以多反应监测模式(MRM)对待测物进行定性和定量分析。除磺胺噻唑(STZ)为3 ng/L外,其余检出限为1 ng/L。加标水样的回收率在22.3%～87.0%之间,采用外标法定量。该方法灵敏度高、选择性好、准确度高,适合实际水样中痕量磺胺类药物的检测。
应用液液萃取高效液相色谱-串联质谱法测定水中的氯霉素残留,流动相为甲醇:水(80:20)。采用负电喷雾离子源,在多反应性监测模式下采集信号,定性离子对为321/121、321/152、321/176,定量离子对为321/152。本方法的线性范围是0.1μg/L～100μg/L,其相关系数为0.9993,方法检出限为10 ng/L,回收率在81.7%～121.0%之间。还建立了超声波辅助萃取,高效液相色谱测定沉积物中的氯霉素残留的方法。
2006年开展中国沿岸陆源抗生素排海浓度分布的调查。排污口水域已经受到磺胺类化合物的药物污染,低于国外地表水的污染水平。但是,随着其大量生产及应用,污染问题也变得越来越严重。城市生活污水排放是入海水域磺胺类污染物的主要来源。在所有54个排污口水样品中,未检出氯霉素残留。对大连近岸海域养殖环境进行调查,在水样品中发现氯霉素残留。
Antibiotics are not only administered worldwide in human and animal medicine for the treatment of infections but are an integral part of modern animal production. After consumption, a great part of antibiotic pharmaceuticals mainly enter the environment unmetabolited and can eventually reach the aquatic environment. Their environmental occurrence and fate is of particular interest, due to the potential spread and maintenance of antibacterial resistance. The research focuses on the sulfonamides and chloramphenicol, which are used frequently as human and animal medicines.
This research developed a rapid method for the determination of 14 kinds of sulfonamides (SAs) in wastewater using solid-phase extraction (SPE), and liquid chromatography tandem mass spectrometry (LC-MS/MS) with positive electrospray ionization (ESI(+)) and multiple reaction monitoring (MRM) mode. The SPE was performed on an Oasis HLB cartridge. Chromatographic separation on a C18 column was achieved using a binary eluent containing methanol and water with 0.2% formic acid. Typical recoveries of the analytes ranged from 22.3% to 87.0% at a fortification level of 100 ng/L. The limits of detection (LOD) in wastewater except sulfathiazole (3 ng/L) could be detected and quantified at levels as low as 1 ng/L.
Chloramphenicol in water was extracted liquid-liquid extraction and determined by HPLC-MS/MS, using methanol-water (80:20) as the mobile phase. The spectral acquisition was done in the negative electron spray ionization utilizing multiple reaction monitoring of three parent- daughter ion pairs: m/z 321/121, 321/152 and 321/176. The ion pair of m/z 321/152 was used for quantitation. Linear plots were obtained between 0.1μg/L and 100μg/L, with linear correlation coefficient of 0.9993. The limit of detection was 10 ng/L. Ultrasonic assistance extraction followed by HPLC analysis was applied for the determination of the concentration in the sediment samples.
In 2006, an antibiotic monitoring campaign was carried out, which focused on the distribution in the coastal zone of China by the discharge of land-based wastewater. The result shows the water occurred the sulfonamide antibiotics' residue. But they are lower than the water pollution level in the developed countries. However, with its large-scale production and application, the problem of pollution is becoming more and more serious. The municipal wastewater discharge is the most important source of sulfonamides in these sites. All 54 water samples have not been detected chloramphenicol residues. For the investigation in aquaculture environment, water samples were found chloramphenicol residues.
引文
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