摘要
由于可能造成细菌抗药性威胁人类健康,抗生素污染成为热门话题.制药废水中残留抗生素的检测对于抗生素污染的控制具有重要意义.采用固相萃取-高效液相色谱法,建立了制药废水中美罗培南、普鲁卡因青霉素、头孢唑林钠3种β-内酰胺类抗生素的同步检测方法.水样经固相萃取后,选用乙酸铵-乙酸和乙腈作为流动相以90%∶10%比例进行高效液相色谱分析.研究了固相萃取柱类型、萃取pH、洗脱溶液体积、液相色谱柱类型、流动相组成及pH、流速的影响.建立的方法对实际水样加标回收率为74.67%~106%,相对标准偏差为0.3%~6.3%,方法定量限为2.65~5.87μg/L.该方法操作简单,准确度高.应用该方法测定了某制药废水进水美罗培南、普鲁卡因青霉素、头孢唑林钠的平均浓度分别为139.7μg/L、75.1μg/L、185.6μg/L,出水平均浓度分别为7.0μg/L、9.9μg/L、18.5μg/L,三种抗生素的去除率分别为95.0%、86.8%、90.1%.该方法可以满足制药企业日常监测分析的要求.
Antibiotics pollution is hot topic nowadays as it may increase antibiotic-resistant bacteria which pose great threat to the human health.The detection of trace antibiotics in pharmaceutical wastewater is important for its pollution control.However,it is difficult as the wastewater is complex which affects the accuracy.An analytical method for the simultaneous detection of three kinds ofβ-lactam antibiotics including meropenem,procaine penicillin,and cefazolin sodium in pharmaceutical wastewater was established by using solid phase extraction and high performance liquid chromatography(HPLC)with ultraviolet detector.The antibiotics were extracted by passing through cartridges,then separated by HPLC process with 90%ammonium acetate-acetic acid and 10%acetonitrile as the mobile phase.The conditions were systematically investigated,such as the type of solid phase extraction column,extraction pH,the volume of eluate,the type of HPLC column,composition and pH and flow rate of the HPLC mobile phase.The results showed that HLB column was better than C18 as the solid phase extraction column.The method was optimized at the extraction pH of 4,methanol elution solution volume of 10 mL,the mobile phase composition of 9%∶1%,the mobile phase pH of 4 and flow rate of 0.4 mL/min.The recovery rate in actual water sample is 74.67%~106%,and the limit of quantification is 2.65~5.87μg/L.This method was simple with good accuracy.It was applied to determine the influent and effluent concentration of meropenem,procaine penicillin,and cefazolin sodium in a pharmaceutical wastewater treatment station,and the value was 139.7μg/L,75.1μg/L,185.6μg/L for theinfluent and 7.0μg/L,9.9μg/L,18.5μg/L for the effluent,respectively.Meanwhile,the removal efficiency of them was determined to be 95.0%,86.8%,and 90.1%,respectively.The method meets the demand of routine detection of the mentioned threeβ-lactam antibiotics and also provides reference to build detection method of other antibiotics.
作者
孔瑜
段锋
吴达
张西华
KONG Yu;DUAN Feng;WU Da;ZHANG Xi-hua(WEEE Research Center, Research Center of Resource Recycling Science and Engineering, Shanghai Polytechnic University,Shanghai Collaborative Innovation Center for WEEE Recycling, Shanghai 201209, China;Beijing Engineering Research Center of Process Pollution Control, Division of Environment Technology and Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China;North China Pharmaceutical Huasheng Co., Ltd., Shijiazhuang 052160, China)
出处
《湘潭大学学报（自然科学版）》
CAS
2021年第4期102-110,共9页
Journal of Xiangtan University(Natural Science Edition)
基金
国家重点研发计划项目(2018YFC1801501)
上海第二工业大学研究生资助项目(EGD19YJ0006)
上海高校知识服务平台项目(ZF1224)。
关键词
制药废水
抗生素
固相萃取
高效液相色谱
检测方法
pharmaceutical wastewater
antibiotics residue
solid phase extraction
high performance liquid chromatography
detection method
