高效液相色谱法测定渔业用水中喹乙醇代谢物残留量

Determination of olaquindox metabolite residue in fishery water by HPLC

建立了固相萃取-高效液相色谱测定渔业用水中喹乙醇代谢物残留量的方法。3-甲基喹噁啉-2羧酸(MQCA)经PAX固相萃取柱纯化和富集,用含2%甲酸的乙酸乙酯溶液洗脱,甲醇和1. 0%甲酸水溶液作为流动相,经C18柱分离,10 min内出峰。MQCA在0. 01～1. 00 mg/m L范围内线性良好,相关系数为0. 999 91,外标法定量,MQCA的检出限为0. 01 mg/L,定量限为0. 02 mg/L,平均加标回收率为79. 0%～99. 3%,相对标准偏差(RSD)为7. 38%～9. 12%。利用该方法对山东省济宁市采煤塌陷区重点养殖区的渔业用水进行分析,8个站位中MQCA组分的含量均低于检出限。本方法适用于检测渔业用水中MQCA的残留,可为渔业环境保护提供技术支持。

A method of high performance liquid chromatography with solid phase extraction, purification and enrichment, followed with eluting with ethyl acetate containing 2% formic acid was established for detection of MQCA in fishery water. The samples were separated by the PAX C 18 column with a mobile phase of methanol and 1.0 % formic acid within 10 minutes. The linearity of MQCA over the concentration range 0.01-1.00 mg/mL was well by the external standard method, and the correlation coefficient was 0.999 91. The detection limit of MQCA was 0.01 mg/L based on the ratio of signal to noise ( S/N =3), and the quantitation limit of MQCA was 0.02 mg/L based on the ratio of signal to noise( S/N =10). The mean recoveries rate ranged from 79.0% to 99.3%, with relative standard deviation in the region of 7.38%-9.12%. The method was used to analyze fishery water from the important aquaculture areas in coal mining subsidence district. Each content of MQCA in the water samples from 8 stations was lower than the detection limit. In conclusion, this method is suitable for the detection of MQCA residues in fishery water, providing technological support for protecting fishery environment.[Chinese Fishery Quality and Standards, 2019, 9(1):64-69].