超快速液相色谱-串联质谱联用法测定蜂蜜中20种痕量磺胺类药物残留研究

Simultaneous determination of twenty trace sulfonamides residues in honey by ultra-fast liquid chromatography coupled with tandem mass spectrometry

目的:建立一种快速、准确、高效、灵敏的同时测定蜂蜜中20种磺胺类药物残留的超快速液相色谱-串联质谱测定方法。方法:蜂蜜样品用0.1%(V/V)磷酸提取后,经MCX固相萃取小柱净化,在快速液相分析色谱柱Shim-packXR-ODSⅡ(100 mm×2.0 mm i.d.,2.2μm)上,以内含0.1%(V/V)甲酸和5 mmol/L乙酸铵的乙腈/水溶液为流动相,采用梯度洗脱。利用超快速液相色谱-三重四级杆串联质谱联用(UFLC-MS/MS)电喷雾电离多反应监测(MRM)正离子模式检测。结果:20种磺胺类药物除磺胺胍和磺胺醋酰外均在0.25μg/kg～25.0μg/kg范围具有良好的线性关系,磺胺胍和磺胺醋酰在1.0μg/kg～25.0μg/kg范围具有良好的线性关系,相关系数>0.99,在0.5μg/kg、2.5μg/kg和5.0μg/kg三个水平添加时,各被测物的回收率在63.3%～106.9%范围,相对标准偏差(RSD)在1.7%～12.3%范围,检出限在0.004μg/kg～0.25μg/kg范围,最低定量检出限在0.01μg/kg～0.83μg/kg范围。结论:建立的方法可在5.5 min内同时测定20种磺胺,是一种蜂蜜中磺胺类药物残留测定的高效快速分析方法,用于实际样品的检测,结果满意。

Objective：To develop a fast,efficient,accurate and sensitive method for determination of sulfonamides residues in honey by ultra-fast liquid chromatography tandem mass spectrometry.Methods： Honey samples were extracted using 0.1%（V/V） phosphoric acid,and purified by MCX solid-phase extraction（SPE） cartridges.The separation was carried out on a Shim-pack XR-ODS Ⅱ（100 mm×2.0 mm i.d.,2.2 μm） with acetonitrile and water as mobile phase by gradient elution,which containing 0.1%（V/V） formic acid and 5 mmol/L ammonium acetate.Detection was performed by an ultra-fast liquid chromatography-triple quadrupole tandem mass spectrometry（UFLC-MS/MS） with an electrospray ion（ESI） source in the positive multipile reaction monitoring（MRM） mode.Results： Calibration curves for the sulfonamides except sulfaguanidine and sulfacetamide were linear within the range of 0.25 μg/kg～25.0 μg/kg,and 1.0 μg/kg～25.0 μg/kg for sulfaguanidine and sulfacetamide.The correlation coefficients were more than 0.99,the limits of detection（LODs）were between 0.004 μg/kg～0.25 μg/kg,and the limits of quantification（LOQs）were between 0.01 μg/kg～0.83 μg/kg.The extraction recoveries ranged from 63.3% to 106.9% at three spiked levels of 0.5 μg/kg,2.5 μg/kg,5.0 μg/kg for each sulfonamide,and the RSDs ranged from 1.7% to 12.3%.Conclusion： The developed method can be detected simultaneously 20 sulfonamides within 5.5 min.It is fast and efficient,and which has used satisfactorily for the determination of trace sulfonamides in actual honey samples.