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作 者:宋佳 赖焕华 蓝献泉 姜丽君 陈华龙 SONG Jia
出 处:《天津化工》2025年第2期108-111,共4页Tianjin Chemical Industry
摘 要:本文建立了一种可同时测定《化妆品安全技术规范》(2015年版)所规定的禁用植物原料鸦胆子中3种苦木内酯(鸦胆苦素A、鸦胆苦素D和鸦胆苦醇)含量的超高效液相色谱-串联质谱法。采用反向色谱系统对这3种苦木内酯进行分离,所使用的色谱柱为SHIMADZUShim-packGIST-HPC18柱(1.9μm,2.1mm×100mm),柱温设定为30℃,流动相以乙腈-0.5%甲酸进行梯度洗脱,流速为0.3mL/min,进样量1μL,3种苦木内酯均运用正离子、多离子反应监测模式。实验结果表明,在各自的浓度范围内,3种苦木内酯的线性相关系数r均大于0.999,呈现出良好的线性关系。在低、高两个浓度水平下的加标回收率分别为97.4%~103.5%(RSD为1.7%~3.4%)以及98.6%~103.6%(RSD为2.0%~3.4%)。当取样量为1g时,该方法的检出浓度范围为0.03~0.15μg/g。综上所述,此方法能够准确且快速地对化妆品禁用植物原料鸦胆子中的3种苦木内酯进行定量分析。An analytical method based on UPLC-MS/MS for the determination of 3 Kinds of Nigakilactone from brucea Javanica was established.The separation was performed on a SHIMADZU Shim-pack GIST-HP C18 column.Acetonitrile and 0.1%formic acid were used as mobile phases with gradient elution at a flow rate of 0.30 mL/min.A triple quadrupole mass spectrometer operating in positive electrospray ionization mode with multiple reaction monitoring was used.The re-sults of 3 Kinds of Nigakilactone show good linear relationships within their own rangers,the correlation coefficients(r)are above 0.999,The recoveries at low and high spiking levels were 97.40%~103.5%,And relative standard devia-tions ranged from 1.7%~3.4%,The limits of detections(LODS)for the 3 kinds of nigakilactone within the range of 0.03~0.15μg/g.This method was efficient,accurate for the deterrmination of Simultaneous Determination of 3 kinds of nigakilactone from prohibited raw materia brucea javanica.
关 键 词:化妆品 超高效液相色谱-串联质谱法 原料 鸦胆子 苦木内酯
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