Xie Min, Xu Jun, Fei Dan, Guang Ye-Lan, Zhou Yao-Min, Li Fan, Hu Li-Zhen
Institute for Quality & Safety and Standards of Agricultural Products Research, Jiangxi Academy of Agricultural Sciences, Key Laboratory of Agro-product Quality and Safety of Jiangxi Province Nanchang Jiangxi China
Animal Husbandry and Veterinary Science of Jiangxi Academy of Agricultural Sciences Nanchang Jiangxi China.
RSC Adv. 2024 Oct 29;14(46):34261-34269. doi: 10.1039/d4ra04330h. eCollection 2024 Oct 23.
An improved QuEChERS method combined with Multi-Plug Filtration Cleanup (m-PFC) clean-up procedure was developed for the simultaneous determination of 16 different sulfonamides in forage grasses using ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS). The forage grass sample was extracted with 0.1 mol L NaEDTA-Mcllvaine buffer and acetonitrile solution, purified by the Navo U-QuE column tube, separated by Agilent ZORBAX Eclipse Plus C column, and analyzed by MRM (multiple reaction monitoring) mode and the internal standard method was utilized for quantification. The 16 different sulfonamides display good linearity within the range of 0.5-50 μg L ( > 0.9967), the limit of detection was 0.02-0.5 μg kg, and the limit of quantification was 0.05-1.0 μg kg. Under the additive amounts of 1, 2, and 10 μg kg, the recoveries were in the range of 72.3-116.9%, and the relative standard deviation was between 1.4% and 10.3%. The presented method showed the advantages of simple operation, excellent selectivity and high sensitivity. It was well-suited for both qualitative and quantitative analyses of sulfonamides in forage grass. Overall, this method provided a scientific basis for risk assessment, enforcement of quality and safety standards, and detection of sulfonamide residues in forage grass for import and export.
建立了一种改进的QuEChERS方法,并结合多插头过滤净化(m-PFC)净化程序,使用超高效液相色谱串联质谱(UHPLC-MS/MS)同时测定牧草中的16种不同磺胺类药物。牧草样品用0.1 mol L NaEDTA-Mcllvaine缓冲液和乙腈溶液萃取,通过Navo U-QuE柱管净化,用安捷伦ZORBAX Eclipse Plus C柱分离,采用多反应监测(MRM)模式分析,以内标法定量。16种不同的磺胺类药物在0.5-50 μg L范围内线性良好(r>0.9967),检出限为0.02-0.5 μg kg,定量限为0.05-1.0 μg kg。在1、2和10 μg kg的添加量下,回收率在72.3-116.9%范围内,相对标准偏差在1.4%至10.3%之间。该方法操作简单、选择性好、灵敏度高,适用于牧草中磺胺类药物的定性和定量分析。总体而言,该方法为牧草中磺胺类药物残留的风险评估、质量安全标准的执行以及进出口检测提供了科学依据。