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作 者:吕琼芳 彭敏[1] 梁惠明[1] 黄少宏[1] 杜瓦 Lv Qiongfang;Peng Min;Liang Huiming;Huang Shaohong;Du Wa(Jiangmen Institute for Drug Control,Jiangmen 529000,China)
机构地区:[1]江门市药品检验所,江门529000
出 处:《分析仪器》2021年第5期24-29,共6页Analytical Instrumentation
基 金:2021年度江门市基础与理论科学研究类科技计划项目(编号:江科[2021]87号)。
摘 要:建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定化妆品中63种激素类组分的优化方法。以Shim-pack XR-ODSⅢC_(18),2.2μm(ID2.0mm×150mm)色谱柱进行分离,以乙腈和水为流动相梯度洗脱,流速为0.3 mL/min,进样量为10μL,柱温:40℃。采用多反应监测(MRM)扫描方式,正负源组分同时检测。以保留时间和特征离子对的相对丰度比定性、定量离子对峰面积定量,以标准曲线计算样品含量。所优化的方法在相应的浓度范围内浓度和峰面积的线性关系良好,线性相关系数均达到0.99以上;定量下限浓度的平均回收率为73.7%~106.3%,相对偏差小于12%,其他浓度回收率为90.8%~118.6%,相对偏差小于6%;检出限、定量限及精密度均符合标准的要求。该方法准确、可靠,适用于化妆品中化妆品中63种激素类组分的同时测定。The separation was carried out on a Shim-pack XR-ODSⅢC_(18),2.2μm(ID2.0mm×150mm)column,with gradient elution using acetonitrile and water as mobile phases.The flow rate was 0.3 mL/min,the injection volume was 10μL,the column temperature was 40℃.The multiple reaction monitoring(MRM)was used to detect both positive and negative source components.In this method,the retention time and relative abundance ratio of characteristic ion pairs were used for qualitative test,the peak area of quantitative ion pairs were used for quantification test,the contents were calculated by standard curve.The linear relationship between concentration and peak area were good in the corresponding concentration range,and the linear correlation coefficients were all above 0.99.The average recoveries of the lower limit of quantitation were between 73.7%and 106.3%,and the relative deviations were less than 12%.The recoveries of other concentrations were between 90.8%and 118.6%,and the relative deviations were less than 6%.The detection limits,quantitation and precision met the requirements of standards.The method is accurate and reliable.
关 键 词:化妆品 激素 63组分 超高效液相色谱-串联质谱法(UPLC-MS/MS)
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