固相萃取-高效液相色谱-串联质谱法同时测定不同基质保健食品中10种减肥药物

摘要

采用固相萃取高效液相色谱-串联质谱法同时测定不同基质保健食品中10种减肥药物.保健食品样品采用甲醇超声提取,经Oasis HLB固相萃取柱净化,以Zorbax-SB-C18色谱柱为分离柱,以不同体积比的10 mmol·L-1乙酸铵-0.1％(体积分数)甲酸溶液和乙腈的混合液为流动相进行梯度洗脱,采用电喷雾正离子源多反应监测模式检测.10种减肥药物的质量浓度均在1.0～100.0μg· L-1内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为1.2～3.8 μg·kg-1.以空白样品为基体进行加标回收试验,所得回收率为79.5％～106％,测定值的相对标准偏差(n=6)为2.5％～9.7％.%HPLC-MS/MS was applied to the simultaneous determination of 10 diet drugs in health-care foods of different matrices with solid phase extraction.The health-care food sample was extracted ultrasonically with methanol,and the extract was purified by Oasis HLB solid phase extraction column.Zorbax-SB-C18 chromatographic column was used as stationary phase,and the mixtures of 10 mmol · L-1 ammonium acetate-0.1％ (ψ) formic acid solution and acetonitrile mixed in different ratios were used as mobile phase in gradient elution.ESI() and multi-reactions monitor mode were adopted in MS/MS.Linear relationships between values of peak area and mass concentration of the 10 diet drugs were kept in the same range of 1.0-100.0 μg · L-1,with detection limits (3S/N) in the range of 1.2-3.8 μg · kg-1.On the base of blank sample,test for recovery was made by standard addition method.Values of recovery found were in the range of 79.5％-106％,with RSD's (n=6) in the range of 2.5 ％-9.7 ％.