液相色谱-高分辨质谱法测定壮阳类保健品中非法添加物
LC-HRMS Determination of Illegal Additives in Impotence Health Products
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摘要: 采用液相色谱-高分辨质谱法检测壮阳类保健品中的5种非法添加物.样品经甲醇超声提取后,以C18色谱柱为分离柱,以0.1%(体积分数)乙酸溶液与乙腈组成的混合溶液为流动相进行梯度洗脱,采用电喷雾正离子源及全扫描/二级质谱目标离子扫描模式进行测定.5种非法添加物的线性范围为1.0~50 μg·L-1,方法测定下限(10S/N)在0.3~0.4 μg·L-1之间.对样品进行加标回收试验,回收率在78.0%~102%之间,测定值的相对标准偏差(n=6)在0.62%~2.3%之间.Abstract: A method of LC-HRMS was used to measure five kinds of illegal additives in impotence health products. The sample was extracted with methanol by untralsonic. The eluate was separated on a C18 column with a the mixture of 0.1% (φ) acetic acid and acetonitrile as mobile phase for gradient elution. ESI+ and full scan MS2 were adopted in HRMS. The linearity ranges of the five kinds of illegal additives were 1.0-50 μg·L-1,with limits of quantification (10S/N) in the range of 0.3-0.4 μg·L-1. Recovery rate measured by standard addition method was in the range of 78.0%-102% with RSD′s (n=6) in the range of 0.62%-2.3%.