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

Simultaneous extraction and determination of nine chemically synthetic anticoccidial drug multi-residues in chicken meat using high performance liquid chromatographytandem mass spectrometry

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、磺胺喹口恶啉、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Hyper-sil 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20～150μg/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 μg/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.