高效液相色谱-串联质谱法检测鸡肉中9种化学合成类抗球虫药多残留

摘要

建立了鸡肉中氯羟吡啶、二硝托胺、4,4’-二硝基均二苯脲(尼卡巴嗪代谢物)、磺胺氯吡嗪、磺胺喹(噁)啉、地克珠利、妥曲珠利、妥曲珠利砜和妥曲珠利亚砜9种化学合成类抗球虫药多残留的高效液相色谱-串联质谱分析方法.样品采用2％乙酸酸化的乙腈/二甲亚砜(4∶1,v/v)提取,150 mg二甲基十八碳硅烷粉(octadecylsilyl,ODS)、100mg石墨化炭黑(graphitized carbon black,GCB)和100 mg弗罗里硅土(Florisil)吸附剂分散固相萃取净化,经Hypersil GOLD C18色谱柱(150 mm×4.6 mm,5μm)分离,电喷雾串联四极杆质谱多反应离子监测方式测定.9种分析物在20～150 μg/kg范围内线性关系良好,相关系数均大于 0.995.样品基质中9种分析物在20、50和150μg/kg加标水平下,平均回收率为81.5％ ～ 103.6％,相对标准偏差为4.5％～14.5％.该方法稳定、可靠,可满足鸡肉中化学合成类抗球虫药多残留的检测与确证.%A high performance liquid chromatography-tandem mass spectrometric (HPLC-MS/ MS) method was developed for the simultaneous extraction and determination of multi-residues of nine chemically synthetic anticoccidial drugs in chicken meat. Toltrazuril-D3 was used as the internal standard. The sample was extracted by 15 mL acetonitrile/dimethyl sulfoxide (4:1, v/ v, containing 2% acetic acid), cleaned-up by a QuEChERS (quick, easy, cheap, effective, rugged and safe) clean-up tube with 150 mg octadecylsilyl (ODS), 100 mg Florisil and 100 mg graphitized carbon black (GCB). After the concentration, the extract was analyzed by HPLC-MS/MS. The results showed that good linearity in the range of 20-150 jig/L for each target compound. The recoveries were between 81.5% and 103.6% with the relative standard deviations lower than 15%. The method is simple, rapid, and suitable to detect the chemically synthetic anticoccidial drug residues with high throughput.