环境水体中磺胺类抗生素分析方法的建立与应用
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摘要
应用高效液相色谱-串联质谱(HPLC-MS/MS)联用的技术,建立了水体中磺胺类抗生素的检测方法。选用电喷雾离子源(ESI),在正离子模式下对目标化合物进行选择性反应检测(SRM)扫描。采用固相萃取法对样品进行前处理,通过HLB小柱对样品进行富集和净化。液相色谱选用C18柱,以甲醇和0.1%甲酸作为流动相对样品进行梯度洗脱分离。方法的回收率为53.6%～96.2%。方法的最低检出限除磺胺噻唑(STZ)为0.3 ng/L外,其余均为0.1 ng/L,本方法的RSD为4.7%～9.3%,该方法适用于水体中磺胺类抗生素的残留检测。
An analysis method for sulfonamide antibiotics in water bodies was established using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) technology. Electrospray ion sources(ESI) were used to scan the target compound in positive ion mode for selective reaction monitoring(SRM). The samples were pretreated by solid phase extraction and enriched and purified by HLB column. C18 column was selected for liquid chromatography, and samples were subject to gradient elution separation using methanol and 0.1% formic acid as moving phases. The recovery rate of the method is 53.6%～96.2%. The lowest detection limit of the method is 0.1 ng/L except that it is 0.3 ng/L for sulfathiazole(STZ), and RSD of the method is 4.7% ～ 9.3%. This method is suitable for the residual detection of sulfonamide antibiotics in water bodies.
An analysis method for sulfonamide antibiotics in water bodies was established using high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) technology. Electrospray ion sources(ESI) were used to scan the target compound in positive ion mode for selective reaction monitoring(SRM). The samples were pretreated by solid phase extraction and enriched and purified by HLB column. C18 column was selected for liquid chromatography, and samples were subject to gradient elution separation using methanol and 0.1% formic acid as moving phases. The recovery rate of the method is 53.6%～96.2%. The lowest detection limit of the method is 0.1 ng/L except that it is 0.3 ng/L for sulfathiazole(STZ), and RSD of the method is 4.7% ～ 9.3%. This method is suitable for the residual detection of sulfonamide antibiotics in water bodies.
引文
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[16]朱学武,成小翔,甘振东,等.饮用水中抗生素去除技术研究进展[J].给水排水,2017,43(5):135-141.
[2] DENG W J,LI N,ZHENG H L,et al.Occurrence and risk assessment of antibiotics in river water in Hong Kong [J].Ecotoxicology and Environmental Safety,2016,125:121-127.
[3] WATKINSON A J,MURBY E J,Kolpin D W,et al.The occurrence of antibiotics in an urban watershed:From wastewater to drinking water [J].Science of the Total Environment,2009,407:2711-2733.
[4] 徐维海,张干,邹世春,等.香港维多利亚港和珠江广州段水体抗生素的含量特征及季节变化[J]环境科学,2006,27(12):2468-2462.
[5]XU W H,ZHANG G,ZOU S C,et al.A Preliminary investigation on the occurrence and distribution of antibiotics in the Yellow River and its Tributaries,China [J].Water Environment Research,2007,81(3):248-252.
[6]ZOU S C,XU W H,ZHANG R J,et al.Occurrence and distribution of antibiotics in coastal water of the Bohai Bay,China:Impacts of river discharge and aquaculture activities [J].Environmental Pollution,2011,159:2913-2920.
[7]Luo Y,Xu X,Rysz M,et al.Occurrence and Transport of Tetracycline,Sulfonamide,Quinolone and Macrolide antibiocis in the Haihe River Basin,China [J].Environ Sci Technol,2011,45(5):1827-1833.
[8 ]Chang X,Meyer M T,Liu X,et al.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 [J].Environmental Pollution,2010,158(5):1444-1450.
[9 ]孙广大,苏仲毅,陈猛,等.固相萃取-超高压液相色谱-串联质谱同时分析环境水样中四环素类和喹诺酮类抗生素[J].色谱,2009,27(1):54-58.
[10]陈敏,万华,徐爱兰,等.长江口地区饮用水源地有毒有害污染状况分析与评价[J].南通大学学报(自然科学版),2011,20(02):41-47.
[11]张俊,罗阳,潘曼曼,等.水体中磺胺、四环素、喹诺酮类抗生素检测方法[J].中国环境监测,2013,29(04) :111-115.
[12]苏仲毅,陈猛,袁东星,等固相萃取-超高压液相色谱-串联质谱法分析海水中 9 种磺胺类抗生素[J].厦门大学学报:自然科学版,2007,46(增刊1):72-76.
[13]徐维海.典型抗生素类药物在珠江三角洲水环境中的分布、行为与归宿[D].广州:中科院广州地球化学研究所,2007.
[14] 南琼,唐景春,胡羽成,等.不同环境介质中抗生素检测方法研究进展[J] ,化学研究与应用,2017,29(11):1609-1621.
[15]陈凯杰.试论饮用水中抗生素去除技术研究进展[J].科技经济导刊 2018,26(8):103-105.
[16]朱学武,成小翔,甘振东,等.饮用水中抗生素去除技术研究进展[J].给水排水,2017,43(5):135-141.