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1. 样品制备:称6g蜂蜜样品+30mL提取液(pH=4.0),旋涡振荡 <G9HVMiP
提取液配制:柠檬酸10.5g+磷酸氢二钠(无水)8.88g+乙二胺四乙酸钠30.3g+820mL水,用2M HCl调pH至4.0) -6Y@
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2.SPE步骤 L701j.7"
①Cleanert PEP(500mg/6mL) ?/M:
活化:甲醇,水 _#UiY
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上样:把样品提取液过柱 diz=|g=w
淋洗:5%甲醇/水 5mL,抽干 NihUCj"
②Cleanert COOH(500mg/3mL) pjN4)y>0
活化:乙酸乙酯,2柱管 `<Q[$z
③Cleanert PEP(上)-COOH(下) 串联 O#do\:(b
淋洗: 15mL乙酸乙酯淋洗,拿下PEP柱,COOH柱抽干(5min) 7BS5Eq B=
洗脱: 流动相(0.01M草酸:乙腈:甲醇=350:100:50)4.5mL 2<T/N
定容: 洗脱液用0.01M草酸定容至5mL,摇匀,过滤膜,UPLC测定。