Chen Yongping, Xia Sudong, Han Xianqin, Fu Zhiru
Tianjin Agricultural Ecological Environment Monitoring and Agricultural Product Quality Testing Center, Tianjin 300221, China.
Tianjin Key Lab of Aqua-Ecology and Aquaculture, Department of Fishery Science, Tianjin Agricultural University, Tianjin 300384, China.
J Anal Methods Chem. 2020 Feb 19;2020:3725618. doi: 10.1155/2020/3725618. eCollection 2020.
A fast-analytical method using simplified extraction has been developed for the simultaneous determination of 42 compounds from 4 different classes of veterinary drugs (amphenicols, triphenylmethane, fluoroquinolones, and sulfonamides) in fish by reverse phase liquid chromatography-tandem mass spectrometry. The selection of extraction reagents was optimized using different types of microfiltration membrane, mobile phase, and LC column. Samples were extracted using 0.4% hydrochloric acid in acetonitrile and ethyl acetate and then were cleaned up using solid-phase extraction Cleanert Alumina N columns (500 mg) and Oasis hydrophilic-lipophilic balance (HLB) cartridges. The chromatographic separation was performed on a XR-ODS C column using a mobile phase of (A) 0.1% formic acid and 2 mM ammonium acetate and (B) 0.1% formic acid acetonitrile at a flow rate of 0.25 mL·min. The results indicated 67.7-112.8% recovery of 42 compounds with an intra- and interday relative standard deviations less than 10%. The limits of quantification for analytes were in the range of 0.3-1.0 g kg for samples which were satisfactory to support future surveillance monitoring. The method applicability was checked by analyzing 30 fish samples collected from local markets. Two fish samples surpassed the established MRL of 100 g kg with values of 104 g kg and 112 g kg.
已开发出一种采用简化萃取的快速分析方法，用于通过反相液相色谱 - 串联质谱法同时测定鱼类中4种不同类别的42种兽药（氯霉素、三苯甲烷、氟喹诺酮和磺胺类）。使用不同类型的微滤膜、流动相和液相色谱柱对萃取试剂的选择进行了优化。样品用乙腈和乙酸乙酯中的0.4%盐酸萃取，然后用固相萃取Cleanert Alumina N柱（500 mg）和Oasis亲水亲脂平衡（HLB）小柱进行净化。色谱分离在XR - ODS C柱上进行，流动相为（A）0.1%甲酸和2 mM乙酸铵，（B）0.1%甲酸乙腈，流速为0.25 mL·min。结果表明，42种化合物的回收率为67.7 - 112.8%，日内和日间相对标准偏差小于10%。分析物的定量限在0.3 - 1.0 μg·kg范围内，该结果足以支持未来的监测，令人满意。通过分析从当地市场采集的30个鱼类样品来检验该方法的适用性。两个鱼类样品超过了100 μg·kg的既定最大残留限量，分别为104 μg·kg和112 μg·kg。
