海水中喹诺酮类抗生素液质联用测定前处理方法的优化

Optimization of pre-treatment method for liquid-mass spectrometry of quinolone antibiotics in seawater

为快速建立海水中喹诺酮类抗生素(fluoroquinolones,FQs)检测前处理方法,准确地检测海南文昌冯家湾FQs的质量浓度,采用正交实验对海水中FQs前处理过程进行分析并与未优化前处理方法的回收率进行对比,同时对文昌冯家湾近岸养殖区海水中的FQs进行检测。结果表明:pH=10、上样流速为10 mL·min^(-1)、洗脱剂用量为8 mL、针式滤膜过滤器填充料使用MCE是正交实验后最优前处理条件;正交实验优化后,FQs回收率为62.31%~124.60%,相对标准偏差为1.15%~9.90%,未优化前处理条件FQs回收率为65.07%~112.83%,相对标准偏差为1.60%~24.88%;2种方法在冯家湾均检测出11种FQs,有6种FQs在12个采样点中均有检出,前处理方法优化后所测冯家湾FQs总质量浓度为81.31~136.07 ng·L^(-1),未优化前处理条件所测冯家湾FQs总质量浓度为74.02~114.89 ng·L^(-1)。通过比较2种前处理方法,发现正交实验优化后的前处理方法能够更准确检测出FQs在海水中的质量浓度,可适用于海水中19种FQs的测定。以上研究结果可为精准检测海洋环境中FQs打下基础,也可为冯家湾FQs的管控提供科学依据。

In order to quickly establish a pretreatment method for fluoroquinolones(FQs) detection in seawater and accurately test the mass concentration of FQs in Fengjiawan, Wenchang, Hainan. The orthogonal experiments were conducted to analyze the pretreatment process of FQs in seawater and compare it with the recovery of the unoptimized pretreatment method, and the FQs in seawater from the nearshore culture area of Fengjiawan, Wenchang were also tested. The results showed that the optimal pretreatment conditions determined by the orthogonal experiment were following: pH=10, the loading flow rate of 10 mL·min^(-1), the amount of eluent of 8 mL, and the use of MCE as the filler of the needle membrane filter. After the optimization of the orthogonal experiment, the recovery of FQs was 62.31%~124.60% with the relative standard deviations of1.15%~9.90%, and the recovery of FQs without the optimized pretreatment conditions was 65.07%~112.83%with the relative standard deviations of 1.60%~24.88%;11 kinds of FQs were detected in Fengjiawan by both methods, 6 kinds of FQs were detected in 12 sampling points, the total mass concentrations of FQs measured in Fengjiawan after optimization of the pretreatment method were 81.31~136.07 ng·L^(-1), the total mass concentrations of FQs measured in Fengjiawan without optimization of the pretreatment condition were74.02~74.02 ng·L^(-1). By comparing the two pretreatment methods, it was found that the optimized pretreatment method after orthogonal experiment could detect the mass concentration of FQs in seawater more accurately and could be feasible for the determination of 19 kinds of FQs in seawater. The above results can lay the foundation for accurate FQs detection in the marine environment, and also provide a scientific basis for the control of FQs in Fengjiawan.