基质辅助激光解吸电离飞行时间质谱用于抗生素分析

Matrix Assisted Laser Desorption Ionization Time-of-Flight Mass Spectrometry for Antibiotic Analysis

结合非晶态聚N-乙烯基咔唑(PVK)和兼具基质和吸附剂功能的单层氧化石墨烯(SLGO)优点,制备复合材料PVK@SLGO作为MALDI-TOF MS基质用于喹诺酮类抗生素正、负双离子模式下检测。通过引入同位素内标ENR-D5,建立一种快速便捷MALDI-TOF MS定量分析牛奶样品中ENR方法,喹诺酮类抗生素在0.000 1~1.0 mg/m L浓度范围内具有良好线性关系(R2=0.999 1),采用0.005, 0.01和0.1 mg/mL添加水平的回收率范围在100.7%~113.6%之间,相对标准偏差为9.05%~14%(n=3),该方法的检出限为0.000 1 mg/mL,定量限为0.005 mg/mL。该方法具有良好的准确性和精密度,抗干扰能力强,灵敏度高,为快速分析食品中抗生素残留提供一种通用方法。

The advantages of amorphous poly(N-vinylcarbazole)(PVK) and monolayer graphene oxide(SLGO), which has both matrix and adsorbent functions, are combined to prepare composite materials PVK@SLGO as matrix assisted laser desorption ionization mass spectrometry(MALDI-TOF MS) matrix. It was used for the detection of quinolone antibiotics in positive and negative double ion mode. In addition, by introducing the isotope internal standard enrofloxacin-D5(ENR-D5),a rapid MALDI-TOF MS method for the quantitative analysis of enrofloxacin(ENR) in milk samples was established, which had a good linear relationship in the concentration range of 0.000 1-1.0 mg/mL(R^(2)=0.999 1). The recoveries at the addition levels of 0.005, 0.01 and 0.1 mg/mL are in the range of 100.7% to 113.6%, with the relative standard deviations of 9.05% to 14%(n=3). The limits of detection and the limits of quantification were 0.000 1 and 0.005 mg/mL respectively. This method had good accuracy and precision, strong anti-interference ability and high sensitivity. A general method for rapid analysis of antibiotic residues in food is provided.