采用超高效液相色谱-质谱法测定饮用水中的14种氟喹诺酮类抗生素的残留量。饮用水样品经Oasis HLB(200 mg/6 mL)固相萃取柱富集。柱上的浓集物用甲醇洗脱,洗脱液以Acquity UPLC BEH C18色谱柱为分离柱,以不同体积比的0.1%(体积分数)甲酸溶液和0.1%(体积分数)甲酸乙腈溶液的混合液为流动相进行梯度洗脱,采用电喷雾正离子模式进行质谱检测。14种氟喹诺酮类抗生素均在一定的质量浓度范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.04~1.8 ng·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在69.2%~85.2%之间,测定值的相对标准偏差(n=6)在4.5%~11%之间。

UPLC-MS was applied to the determination of residual amounts of 14 fluoroquinolone antibiotics in drinking water. The sample was passed through Oasis HLB (200 mg/6 mL) SPE column to enrich the fluoroquinolone antibiotics which were eluted from the SPE column with methanol. The eluate was then separated by using Acquity UPLC BEH C18 chromatographic column as stationary phase, and mixtures of (φ) 0.1% formic acid solution and (φ) 0.1% formic acid-acetonitrile solution (mixed in various ratios) as mobile phase in gradient elution. ESI+ was adopted in MS. Linear relationships between values of peak area and mass concentration of the 14 fluoroquinolone antibiotics were kept in definite ranges. Detection limits (3S/N) found were ranged from 0.04 to 1.8 ng·L-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 69.2%-85.2%, with RSD′s (n=6) in the range of 4.5%-11%.