SinChERS结合超高效液相色谱-串联质谱法同时测定禽类产品中磺胺类药物及其增效剂

Simultaneous determination of sulfonamides and sulfonamide potentiators residues in poultry products by SinChERS combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  SinChERS  超高效液相色谱-串联质谱法  禽类产品  磺胺类药物  磺胺增效剂

英文关键词:SinChERS  ultra performance liquid chromatography-tandem mass spectrometry  poultry products  sulfonamides  sulfonamide potentiators

中文摘要:

      目的 建立SinChERS结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography -tandem mass spectrometry, UPLC-MS/MS)同时测定禽类产品中磺胺类药物及其增效剂的分析方法。方法 样品经甲酸乙腈提取后, 经基质分散净化装置(SinChERS)净化, 采用Agilent SB RRHD C18色谱柱(100 mm× 2.1 mm, 1.8 μm)进行分离, 以0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相进行梯度洗脱, 质谱采集采用电喷雾正离子模式, 通过多反应监测(multiple reaction monitoring, MRM)方式检测。结果 磺胺类药物及其增效剂在1~50 μg/L浓度范围内线性关系良好, 相关系数(r2)为0.9994~0.9999。在1.0、2.0、10.0 μg/kg 3个添加水平下, 其平均回收率均在70.2%~99.5%之间, 相对标准偏差(relative standard deviations, RSDs)均小于等于8.6%, 方法定量限为1.0 μg/kg。结论 该方法快速简便、准确可信、灵敏度高, 适合禽类产品中磺胺类药物及其增效剂的残留检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of sulfonamides and sulfonamide potentiators residues in poultry products by SinChERS combined with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The samples were extracted by formic acid-acetonitrile, purified by a novel pressing of the SinChERS packing column, separated by Agilent SB RRHD C18 column (100 mm×2.1 mm, 1.8 μm) with 0.1% formic acid-water and 0.1% formic acid-acetonitrile as mobile phases for gradient elute, then analyzed by UPLC-MS/MS. The determination was carried out with electrospray ion source under the positive ion mode and multiple reaction monitoring (MRM) mode. Results The calibration curves of the sulfonamides and sulfonamide potentiators showed an excellent linearity in the range of 1?50 μg/L, the correlation coefficient (r2) were between 0.9994 and 0.9999. The average recoveries were between 70.2%?99.5% at 3 spiked levels of 1.0, 2.0 and 10.0 μg/kg. The relative standard deviations (RSDs) were less than or equal to 8.6%. The limits of quantitation for the sulfonamides and sulfonamide potentiators were 1.0 μg/kg. Conclusion The proposed method is efficient, reliable and sensitive, which can be used for the detection of sulfonamides and sulfonamide potentiators residues in poultry products.