超高效液相色谱-串联质谱法同时检测消毒产品中13种抗生素

目的采用超高效液相色谱-串联质谱技术,建立消毒产品中8类13种抗生素的检测方法。方法样品经甲醇或乙腈提取后,经Waters HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,三重四级杆串联质谱仪检测。结果13种选定的抗生素在4~100μg/L范围内线性关系良好,相关系数均大于0.991,检出限为2~25μg/kg。在3种不同剂型的消毒产品中,低、中、高3个浓度加标水平的回收率为71.2%~130.4%,相对标准偏差均小于11.3%,满足消毒产品中抗生素违法添加的检测要求。运用建立的方法,在一份膏霜剂型的消毒产品中检测出氧氟沙星,含量为21.1 mg/kg,其余样品中均未检出相关物质。结论该方法简单、可靠、重现性好,覆盖的抗生素种类多。

Simultaneous determination of 13 antibiotics in disinfection products by ultra-high performance liquid chromatography-tandem mass spectrometry

OBEJECTIVE To develop a method for the determination of 13 antibiotics in 8 classes for desinfection products by ulta-high perfomance chromatography-tandem mass spectrometry(UPLC-MS/MS).METHODS Samples were extracted by methanol or acetonitrile.The target compouds were separated on a Waters HSS T3 column(100 mm×2.1 mm,1.8μm),and detected by triple quadrupole tandem mass spectrometer.RESULTS The 13 selected antibiotics showed good linear relationships in the range of 4-100μg/L and the correlation coefficients(r^2)were all above 0.991.The limits of detection ranged from 2 to 25μg/kg.The recovery rates at three spiked levels(low,medium and high)in three dosage forms of disinfection products were in the range of 71.2%-130.4%,and the relative standard deviations(RSD)were all less than 11.3%,which could meet the detection requirements of illegal addition of antibiotics in disinfection products.Ofloxacin at a concentration of 21.1 mg/kg was found in a cream disinfection product by the developed method,and no related drugs were detected in other samples.CONCLUSION This method is simple,reliable,reproducible,which covers a wide range of antibiotics,and provides technical support for monitoring the illegal addition of antibiotics in disinfection products.