超高效液相色谱联质语质中多肽类抗生素

Determination of Peptide Antibiotics in Water by Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

使用0.45μm微孔滤膜过滤水样,然后加入Na2EDTA盐,除去部分金属离子,再调节pH值为3,使用Oasis HLB固相萃取柱富集净化,用5 mL、0.1%的甲酸甲醇和5 mL甲醇洗脱,经氮吹浓缩,以0.1%的甲酸乙腈和0.1%的甲酸水溶液为流动相,采用超高效液相色谱-串联质谱检测多肽类抗生素。检测结果表明,在标准曲线浓度范围内,11种多肽类抗生素线性关系r2均大于0.998,检测限均低于1 ng/L,进行低、中、高浓度加标,平均加标回收率在77.7%~98.1%之间,相对标准偏差在1.5%~14.2%之间。该方法操作简便、测试时间短、准确度和精确度好、检出限低,可以同时测定水质中11种多肽类抗生素。

Water samples were filtered using a 0.45μm pore size membrane,followed by the addition of Na2EDTA salt to remove certain metal ions and pH adjustment to 3.Oasis HLB solid-phase extraction columns were employed for enrichment and purifi cation,with elution using 5 mL of 0.1%formic acid in methanol and 5 mL of methanol.The samples were then concentrated using nitrogen blowdown.Ultra-high-performance liquid chromatography-tandem mass spectrometry was utilized for the detection of peptide antibiotics using a mobile phase consisting of 0.1%formic acid in acetonitrile and 0.1%formic acid in water.The results showed that within the concentration range of the standard curve,all 11 peptide antibiotics exhibited linear relationships with r2 values greater than 0.998,and the detection limits were below 1 ng/L.Low,medium,and high concentration spikes yielded average recoveries ranging from 77.7%to 98.1%,with relative standard deviations ranging from 1.5%to 14.2%.This method is characterized by its simplicity,short testing time,good accuracy and precision,and low detection limits.It allows for the simultaneous determination of 11 peptide antibiotics in water quality.