液相色谱-串联质谱法测定护肤类化妆品中5种棕榈酰多肽

LC-MS/MS Determination of 5Palmitoyl Polypeptides in Skin-Care Cosmetics

护肤类化妆品样品用含0.1mol·L^(-1)乙酸铵的95%(体积分数)甲醇溶液提取,提取液经滤膜过滤后,采用液相色谱-串联质谱法测定滤液中5种棕榈酰多肽的含量。以LIChrospher?60RP-select B色谱柱为固定相,以不同体积比的含0.3%(体积分数)乙酸的50mmol·L^(-1)乙酸铵溶液和乙腈的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源正、负离子模式和选择反应监测模式。5种棕榈酰多肽的质量浓度均在2.0~200.0μg·L^(-1)内与其对应的峰面积呈线性关系,测定下限(10S/N)均为2.0μg·L^(-1)。以空白样品为基体进行加标回收试验,所得回收率为89.4%~111%,测定值的相对标准偏差(n=6)为1.1%~10%。

The sample of skin-care cosmetic was extracted with 95%(volume fraction)methanol solution containing 0.1mol·L^(-1) ammonium acetate,and then the extract was filtered on filter membrane.LC-MS/MS was applied to the determination of 5palmitoyl polypeptides in the filtrate.LIChrospher?60RP-select B chromatographic column was used as stationary phase,and the mixture of 50mmol·L^(-1) ammonium acetate solution containing 0.3%(volume fraction)acetic acid and acetonitrile mixed in different ratios was used as mobile phase in gradient elution.ESI+,ESI-and selected reaction monitor mode were adopted in MS/MS.Linear relationships between values of peak area and mass concentration of 5palmitoyl polypeptides were kept in the same range of 2.0-200.0μg·L^(-1),with the same lower limits of determination(10S/N)of 2.0μg·L^(-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 89.4%-111%,with RSDs(n=6)of determined values in the range of 1.1%-10%.