SPE-RRLC-MS/MS法测定制药废水中青霉素G

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。

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

A method based on solid phase extraction-rapid resolution liquid chromatography-tandem mass spectrometry(SPERRLC-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 C 18 RRLC using 0.01 mol / L ammonium acetate solution(0.1% 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 μg / 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 μg / L,1.0 μg / L and 2.0 μg / 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.