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Position: Home > Articles > Determination of Kasugamycin in Brown Rice by HILIC–MS/MS Modern Agrochemicals 2012 (6) 40-42

亲水作用液相色谱串联质谱法测定糙米中春雷霉素残留量

作  者:
刘进玺;钟红舰;董小海;张玲
单  位:
农业部农产品质量监督检验测试中心(郑州)
关键词:
春雷霉素;残留;糙米;亲水作用液相色谱–质谱/质谱
摘  要:
建立了糙米中春雷霉素残留量的亲水作用色谱–质谱联用测定方法。样品用甲醇+水(体积比为9∶1)提取,经HLB和SCX固相萃取小柱净化,以HWaters HPLC BEH HILIC色谱柱H(50mm×2.1 mm,1.7 m)分离,采用UPLC–MS/MS多反应监测(MRM)正离子模式测定,外标法定量。春雷霉素最低检测浓度为0.005 mg/kg,在0.005,0.050,0.100 mg/kg 3个添加水平下,平均回收率为74.9%~82.7%,相对标准偏差为4.9%~6.9%。
译  名:
Determination of Kasugamycin in Brown Rice by HILIC–MS/MS
作  者:
LIU Jin-xi,ZHONG Hong-jian,DONG Xiao-hai,ZHANG Ling(Zhengzhou Centre of Inspection and Testing for Agricultural Products,Ministry of Agriculture,Zhengzhou 450002,China)
关键词:
kasugamycin;residue;brown rice;hydrophilic interaction liquid chromatography-mass spectrometry/mass spectrometry(HILIC-MS/MS)
摘  要:
A method of determination for kasugamycin in brown rice by HILIC-MS/MS was established.The analytes were extracted from samples using methanol and water(V/V,9∶1),and purified with HLB and SCX solid phase extraction columns,then analyzed using UPLC-MS/MS multiple reaction monitoring(MRM) mode via positive electrospray ionization with a Waters HPLC BEH HILIC column(50 mm×2.1 mm,1.7 ?m) as the analytical column.All the analytes were quantified by the external standard method.The limit of quantification was 0.005 mg/kg.The results showed that the average recoveries at the fortified levels of 0.005,0.050,0.100 mg/kg ranged from 74.9% to 82.7%,and the RSD were 4.9%-6.9%.

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