在线固相萃取-超高效液相色谱-三重四级杆质谱法测定地表水中22种磺胺类抗生素

Determination of 22 Sulfonamide Antibiotics in Surface Water by On-line Solid Phase Extraction with Ultra-performance Liquid Chromatography-triple Quadrupole Mass Spectrometry

建立了在线固相萃取-超高效液相色谱-三重四级杆质谱法测定地表水中22种磺胺类抗生素的方法。水样经滤膜过滤,加入0.1%甲酸混匀后采用在线固相萃取柱富集纯化,超高效液相色谱-三重四级杆质谱测定,外标法定量。优化了液相色谱流动相和质谱条件,22种磺胺类抗生素在线性范围内线性良好,相关系数r^(2)大于0.9912;方法检出限为0.04~0.42 ng/L,测定下限为0.16~1.68 ng/L;实际水样低、中、高浓度的平均加标回收率范围为70%~111%;相对标准偏差小于5.7%。该方法与传统离线固相萃取法比较具有简单快速、灵敏度高、样品消耗量小等优点,能用于地表水中22种痕量磺胺类抗生素的测定。

A method was developed for the determination of 22 sulfonamide antibiotics in surface water by online solid phase extraction-ultra performance liquid chromatography-triple quadrupole mass spectrometry. The collected water samples were filtered through the filter membrane, mixed with 0.1 % formic acid,enriched and purified by on-line solid phase extraction column, determined by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry,and quantified by external standard method. After optimization of the mobile phase of liquid chromatography and mass spectrometry conditions, good linearity was observed for all the 22 sulfonamide antibiotics, with a correlation coefficient(r^(2)) greater than 0.9912. The method detection limits were 0.04~0.42 ng/L, and minimum quantitative detection limits were 0.16~1.68 ng/L. The average recoveries of low, medium and high concentrations of actual water samples ranged from 70 % to 111 %. The relative standard deviation is less than 5.7 %. Compared with the traditional off-line solid phase extraction method, this method is simple, rapid, high sensitivity, low sample consumption and can be used for the determination of 22 trace sulfonamide antibiotics in surface water.