摘要
分别采用高效液相色谱/串联质谱法(HPLC-MS/MS)和高效液相色谱法(HPLC)对水产品中的诺氟沙星、环丙沙星和恩诺沙星喹诺酮类药物进行检测,旨在根据检测要求选择最佳的检测方法。通过分析检测限、线性范围、加标回收、精密度和方法比较2种检测方法,同时对22例市售水产品进行检测并比较分析。HPLC-MS/MS法检测灵敏度高于HPLC法,且可快速、准确进行水产品中喹诺酮类药物检测。两种方法对恩诺沙星检测结果的相关系数为0.969,但HPLC检测数据低估于HPLC-MS/MS的2%。由于HPLC-MS/MS检测成本高,因此HPLC法可作为水产品中喹诺酮类药物残留检测的初步筛检方法,而HPLCMS/MS法能准确定量水产品中喹诺酮类药物含量。
Quinolones which have demonstrated broad -spectrum activity against many pathogenic Gram -negative and Gram -positive bacteria are effective antibacterial drugs widely used against various important diseases of livestock and farmed fish. The European Union has established maximum residue limits （ MRL） for quinolone residues in animal tissues because of growing problem of microbial resistance. Thus, the estab-lishment of effective detection methods is required in order to control these drugs. Many papers have been published about the analysis of quinolone residues in animal products. High performance liquid chromatogra-phy/tandem mass spectrometry method （ HPLC - MS/MS ） and high performance liquid chromatography （ HPLC） method which are generally used were applied respectively to detect norfloxacin, ciprofloxacin and enrofloxacin in aquatic products because of their specificity, sensitivity, rapidity and robustness. The pur-pose of this paper was to select the suitable analytical method according to the requirement. The two methods had their own characteristics and were compared with regard to the detection limit, linear range, recovery, precision and influence factors of detection. Paired measurements were also applied to the analysis of commer-cially available 22 aquatic products. HPLC results were evaluated by comparison with the HPLC-MS/MS a-nalysis. The results showed that compared with HPLC, the detection sensitivity of HPLC-MS/MS was high-er. The use of HPLC-MS/MS could realize rapid, sensitive and accurate detection. HPLC results compared with HPLC-MS/MS data showed to underestimate enrofloxacin content of about 2% and a correlation coeffi-cient of 0. 969 was calculated between the two methods. HPLC method is simple and rapid, and its perform-ance could meet the requirements of the domestic and international legislation. HPLC analytical method which is provided for basic food safety inspection agencies in the routine analysis is suitable for preliminary screening of quinolones, while HPLC-MS/MS could be a more accurate quantitative determination method for measur-ing quinolones content in aquatic products for the reason that detailed structure information is provided by mass spectrometry.
出处
《福建水产》
2015年第5期378-385,共8页
Journal of Fujian Fisheries
作者简介
王丽娟（1980-），女，助理研究员，研究方向为水产品质量安全和渔业环境监测研究．E—mail：wangguoqinli@163．com
