A LC-MS/MS method was established for the determination of streptomycin and dihydrostreptomycin in milk.The chromatographic analysis was performed on BEH C18 column of 50 mm×2.1 mm,1.7 μm with a mobile phase con...A LC-MS/MS method was established for the determination of streptomycin and dihydrostreptomycin in milk.The chromatographic analysis was performed on BEH C18 column of 50 mm×2.1 mm,1.7 μm with a mobile phase consisting of 20 mmol/L HFBA acetonitrile and 20 mmol/L HFBA as at flow rate of 0.3 mL/min under 30 ℃.Mass spectrometry was run under positive ESI and MRM mode.The calibration curve showed a good linearity between the peak areas and the concentrations from 0.05 to 2 mg/L with R2 more than 0.998.The of detection limit of the method was 2.5 μg/kg,and the limit of quantification was 5 μg/kg.The average recoveries from spiked milk at the three concentration levels of 50,100 and 200 μg/kg ranged from 83%-113%.The intra-and inter-batch variation coefficients were range of 1.8%-8.9% and 2.4%-12.2%,respectively.展开更多
建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0-500 ng...建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0-500 ng/m L质量浓度范围内链霉素和双氢链霉素呈线性相关,相关系数为0.9999和0.9994,回收率在78.3%-105.9%之间,相对标准偏差在3.1%-6.6%之间。方法采用碱性氧化铝基质分散固相萃取,除去样液中油脂同时也降低样液中酸的浓度,进而降低固相萃取上样液中碱金属离子强度,提高了链霉素和双氢链霉素残留检测的绝对回收率。展开更多
文摘A LC-MS/MS method was established for the determination of streptomycin and dihydrostreptomycin in milk.The chromatographic analysis was performed on BEH C18 column of 50 mm×2.1 mm,1.7 μm with a mobile phase consisting of 20 mmol/L HFBA acetonitrile and 20 mmol/L HFBA as at flow rate of 0.3 mL/min under 30 ℃.Mass spectrometry was run under positive ESI and MRM mode.The calibration curve showed a good linearity between the peak areas and the concentrations from 0.05 to 2 mg/L with R2 more than 0.998.The of detection limit of the method was 2.5 μg/kg,and the limit of quantification was 5 μg/kg.The average recoveries from spiked milk at the three concentration levels of 50,100 and 200 μg/kg ranged from 83%-113%.The intra-and inter-batch variation coefficients were range of 1.8%-8.9% and 2.4%-12.2%,respectively.
文摘建立了不使用离子对试剂,液质联用技术检测鳗鱼中链霉素和双氢链霉素残留量的检测方法。样品经三氯乙酸溶液提取,碱性氧化铝快速净化,弱阳离子交换柱固相萃取,CAPCELL PAK ST柱分离。链霉素和双氢链霉素检出限为1.5μg/kg,在10.0-500 ng/m L质量浓度范围内链霉素和双氢链霉素呈线性相关,相关系数为0.9999和0.9994,回收率在78.3%-105.9%之间,相对标准偏差在3.1%-6.6%之间。方法采用碱性氧化铝基质分散固相萃取,除去样液中油脂同时也降低样液中酸的浓度,进而降低固相萃取上样液中碱金属离子强度,提高了链霉素和双氢链霉素残留检测的绝对回收率。
