超高效液相色谱-电喷雾电离-串联质谱法测定猪粪便中6种抗生素残留的基质效应研究

基质效应普遍存在于液质联用分析中。该文通过评价"离子抑制率"指标,系统考察了应用超高效液相色谱-电喷雾电离-串联质谱法(UPLC-ESI-MS/MS)测定猪粪便中二甲氧苄啶、磺胺对甲氧嘧啶、恩诺沙星、环丙沙星、金霉素、泰乐菌素6种抗生素残留的基质效应。样品经McIlvaine-Na_2EDTA缓冲溶液提取后,采用HLB固相萃取柱净化,浓缩富集后用0.1%甲酸-甲醇溶液(85∶15,体积比)溶解。经SB C_(18)RRHD色谱柱分离,以甲醇-0.1%甲酸为流动相进行梯度洗脱,在正离子电喷雾下采用多反应监测模式检测。结果表明,猪粪便基质对6种抗生素的测定存在基质增强效应。采用基质匹配标准曲线校正法并优化样品处理条件可以对基质效应产生的影响进行补偿与消除。该研究为提高检测结果的准确度与精密度提供了借鉴。

Study on Matrix Effects in Analysis of Six Antibiotics in Swine Manure by Ultra Performance Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry

Matrix effects are universal phenomena in analysis of liquid chromatography-mass spectrometry.By evaluating'Ion suppression',matrix effects of diaveridine,sulfameter,ciprofloxacin,enrofloxacin,chlorotetracycline and tylosin in swine manure detected by ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) were systematically investigated.The sample was extracted with McIlvaine-Na2EDTA buffer solution,purified and concentrated by a HLB Extraction Cartridge.The residue was dissolved by 0.1％ formic acid-methanol(85 ∶ 15,by volume).The target compounds were separated on an SB C18 RRHD chromatographic column with 0.1％ formic acid-methanol as mobile phase by gradient elution and detected in multiple reaction monitoring (MRM) mode via positive electrospray ionization (ESI +).The result showed that matrix enhancement effects existed in the detection of six antibiotics in swine manure.Furthermore,matrix-matched calibration curve and modified sample treatment could be used to compensate or eliminate the matrix effects in analysis of six antibiotics in swine manure.The study provided a reference for improving the accuracy and precision of the detection result.