通过式固相萃取-液相色谱-串联质谱法快速测定中兽药制剂中硝基呋喃类药物

Rapid Determination of Nitrofurans in Traditional Chinese Medicine for Animals by Liquid Chromatography-Tandem Mass Spectrometry with a Through-type Solid-phase Extraction

建立了通过式固相萃取-液相色谱-串联质谱法测定中兽药制剂中硝基呋喃类药物的方法。样品采用乙腈超声提取,PRiME HLB固相萃取柱净化,经Waters BEH C_(18)色谱柱(100 mm×2.1 mm,1.7μm)分离,以甲醇和水为流动相进行梯度洗脱。质谱采用正负离子切换同时扫描,多反应监测(MRM)模式进行分析。结果表明,4种化合物在各自质量浓度范围内线性关系较好,相关系数(r)为0.9958~0.9993。呋喃它酮的检出限为0.4μg/kg,定量限为1μg/kg,呋喃唑酮、呋喃妥因、呋喃西林的检出限均为4μg/kg,定量限为10μg/kg。待测物在10、20、100.0μg/kg(呋喃它酮为1.0、2.0、10.0μg/kg) 3个浓度水平下平均回收率在72.6%~109.7%之间,相对标准偏差为3.5%~10.3%。该方法可用于中兽药制剂中硝基呋喃类药物的测定。

A method was developed for the rapid detection of nitrofurans in traditional chinese medicine for animals by liquid chromatography-tandem mass spectrometry(LC-MS/MS).The samples were ultrasonically extracted with acetonitrile,then cleaned up with a PRiME HLB column.The targets were separated on a Waters BEH C_(18) column(100 mm×2.1 mm,1.7 μm) with methanol and water as mobile phase by gradient elution.The mass spectrometer was operated using positive and negative switching under multiple reaction monitoring(MRM) mode.Results showed that there were good linear relationships for the four analytes in their respective concentration ranges with correlation coefficients(r) of 0.9958-0.9993.The limits of detection and limits of quantification of furaltadone were 0.4 μg/kg and 1 μg/kg,respectively.The limits of detection and limits of quantification of furazolidone,nitrofurantoin and nitrofurazone were 4 μg/kg and 10 μg/kg,respectively.The Average recoveries were in the range of 72.6%-109.7% with the concentration levels at 10,20,and 100 μg/kg for three nitrofurans and 1,2 and 10 μg/kg for furaltadone.The relative standard deviations were range from 3.5% to 10.3%.The proposed method can be applied to simultaneous identification and quantification of nitrofurans in traditional chinese medicine for animals.