建立了液相色谱-电喷雾串联质谱同时测定猪尿液中β-受体激动剂类、激素类、硝基咪唑类和镇静剂类等23种违禁药物多残留分析方法。猪尿试样真空冷冻干燥后,采用Anpel MCX固相萃取小柱净化,经CNW Athena C18色谱柱(150 mm×2.1 mm,5μm)分离,多反应监测模式下进行定性与定量分析。采用基质匹配标准溶液校正,23个药物响应值与其相应质量浓度在0.5~100μg/L范围内呈良好的线性关系,相关系数(r)大于0.99;以3倍和10倍信噪比计算得到的方法检出限和定量限分别为0.5~4.0μg/L和1.0~10μg/L;在4个添加水平定量限、10、20及50μg/L,猪尿中23种药物的平均回收率为50.2%~97.7%;日内相对标准偏差(RSD)小于10%,日间RSD小于18%。应用此方法检测200批次不同来源猪尿,其中2批次检测出克伦特罗,浓度为4.45和2.16μg/L。
A liquid chromatography-electrospray ionization tandem mass spectrometric(LC-ESI-MS/MS) method was developed for the simultaneous determination of 23 forbidden drugs including β-agonists,steriods,nitroimidazoles,sedatives etc.in swine urine.The samples were freeze-dried under vacuum and then dissolved with 10% methanol in water containing 0.1% formic acid,followed by cleanup and enrichment using Anpel MCX solid phase extraction cartridge.Qualitative and quantitative analysis was achieved for the analytes under the multiple reaction monitoring(MRM) mode after the chromatographic separation on a CNW Athena C18(150 mm × 2.1 mm i.d.,5 μm) column.Matrix-matched calibration curves with good correlation coefficients(r0.99) were obtained in the concentration range of 0.5-100 μg/L.The limits of detection(LODs) and the limits of qualification(LOQs) for the 23 compounds were in the range of 0.5-4.0 μg/L(S/N3) and 1.0-10 μg/L(S/N10),respectively.The mean recoveries at the four spiked levels of 1.0-50 μg/L were between 50.2% and 97.9% with the intra-day relative standard deviation(RSD) less than 10% and inter-day RSD less than 18%.The proposed method was successfully used to detect 23 banned drugs in 200 swine urine samples,two of them contained clenbuterol,with the concentrations of 4.45 and 2.16 μg/L,respectively.