SPE-RRLC-MS/MS法测定制药废水中青霉素G  

DETERMINATION OF PENICILLIN G IN PHARMACEUTICAL WASTEWATER BY SPE-RRLC-TANDEM MS

作　　者：李再兴[1,2] 张非非[1] 左剑恶[2] 王勇军 陈平 周崇晖 余忻[2] 

机构地区：[1]河北科技大学环境科学与工程学院,石家庄050018 [2]清华大学环境学院,北京100084 [3]华北制药集团有限责任公司环境保护研究所,石家庄050015

出　　处：《环境工程》2013年第3期135-138,共4页Environmental Engineering

基　　金："十一五"国家水体污染控制与治理科技重大专项(2008ZX07529-006);河北省重大技术创新项目(12276703Z)

摘　　要：建立了利用固相萃取-高分离度快速液相色谱-串联质谱(SPE-RRLC-MS/MS)测定制药废水中青霉素G残留的方法。水样以30%硫酸锌+20%亚铁氰化钾作为沉淀剂沉淀蛋白质后,上清液采用Oasis HLB固相萃取柱富集和净化,以0.01 mol/L乙酸铵溶液(加0.1%甲酸)+乙腈作为流动相进行等度洗脱,经Agilent Plus C18柱分离后,在串联质谱ESI(+)源下进行MRM检测。该方法的青霉素G检出限(S/N=3)为0.02μg/L,目标物在0.0020～1.0 mg/L范围内线性关系良好,线性相关系数为0.9997。在0.20,1.0,2.0μg/L添加水平平均回收率为74.6%～101.4%,相对标准偏差为4.49%～8.17%。该方法灵敏度高、重现性好、定性定量准确,可满足制药废水中青霉素G残留检测的要求。A method based on solid phase extraction-rapid resolution liquid chromatography-tandem mass spectrometry （SPE- RRLC-MS/MS） was developed to determine penicillin G in pharmaceutical wastewater. Water samples were firstly purified through protein precipitation processes with 30% zinc sulfate and 20% potassium ferrocyanide, and then the penicillin G was enriched and purified with Oasis HLB SPE, separated through Agilent Plus Cls RRLC using 0. 01 mol/L ammonium acetate solution（O. 1% formic acid） and acetonitrile as mobile phase, and detected by mass spectrometry in positive ion mode with multiple reaction monitoring （MRM） using an electrospray ionization interface. The detection limit（S/N = 3 ） was 0. 02 p,g/ L. The linear range was 0. 0020mg/L to 1.0 mg/L, with a correlation coefficient of 0. 9997. The recoveries at the spiked concentration of 0.20 υg/L, 1.0 υg/L and 2.0 υg/L ranged from 74. 6% to 101.4% , with a relative standard deviation from 4.49% to 8.17%. The procedure provides a rapid, reliable and sensitive method for determination of penicillin G in pharmaceutical wastewater.

关 键 词：青霉素G 高分离度快速液相色谱-串联质谱 固相萃取 制药废水 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]