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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 d8wVhZKI"
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) 2@<_,'
2.SPE步骤 &>,;ye>A
①Cleanert PEP(500mg/6mL) <\~v$=G
活化:甲醇,水 *9^8NY]
上样:把样品提取液过柱 IR6W'vA
淋洗:5%甲醇/水 5mL,抽干 Sfz
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②Cleanert COOH(500mg/3mL) F@i>l{C
活化:乙酸乙酯,2柱管 4,I,f>V
③Cleanert PEP(上)-COOH(下) 串联 ^ `y7JXI:
淋洗: 15mL乙酸乙酯淋洗,拿下PEP柱,COOH柱抽干(5min) _x,X0ncv]@
洗脱: 流动相(0.01M草酸:乙腈:甲醇=350:100:50)4.5mL |
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定容: 洗脱液用0.01M草酸定容至5mL,摇匀,过滤膜,UPLC测定。