摘要
建立了一种同时测定精油类化妆品中31种生物碱的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法。样品以含有2%甲酸的甲醇-水(3∶1,体积比)为提取溶剂,正己烷除脂;采用HPH-C18色谱柱(2.7μm,100 mm×2.1 mm)分离,以0.2%甲酸水溶液-乙腈为流动相梯度洗脱,流速为0.35 mL/min,在电喷雾正离子模式下以多反应监测(MRM)方式测定。结果表明:31种生物碱在相应的质量浓度范围内线性关系良好,相关系数(r)为0.9928~1.0000。方法检出限为0.09~3.03μg/kg,定量下限为0.31~10.12μg/kg,3个加标水平下的回收率为63.3%~126%,相对标准偏差为0.73%~17%。该方法前处理简便高效,测定结果准确,灵敏度高,适用于精油类化妆品中生物碱的检测及化妆品的安全性评价。
A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS)method was developed for the simultaneous determination of 31 alkaloids in essential oil cosmetics.A mixture of methanol-H2O(3∶1,by volume)containing 2%formic acid solution was selected as extracting agent.Meanwhile,n-hexane was adopted for defatting treatment.The chromatographic separation was performed on an HPH-C18 column(2.7μm,100 mm×2.1 mm)by gradient elution,with water containing 0.2%formic acid-acetonitrile as mobile phases at a flow rate of 0.35 mL/min.The 31 alkaloids were analyzed in positive electrospray ionization mode under multiple reaction monitoring(MRM)mode.Results showed that there were good linear relationships for the analytes in corresponding concentration ranges,with their correlation coefficients(r)of 0.9928-1.0000.The limits of detection(LOD)and limits of quantitation(LOQ)of the method were in the ranges of 0.09-3.03μg/kg and 0.31-10.12μg/kg,respectively.The recoveries at three spiked levels ranged from 63.3%to 126%,with relative standard deviations(RSD)of 0.73%-17%.The method was rapid,accurate and sensitive,and was suitable for the detection of alkaloids in cosmetics and evaluation of safety of cosmetics.
作者
吕小会
罗辉泰
黄晓兰
吴惠勤
霍延平
张秋炎
朱志鑫
LV Xiao-hui;LUO Hui-tai;HUANG Xiao-lan;WU Hui-qin;HUO Yan-ping;ZHANG Qiu-yan;ZHU Zhi-xin(School of Chemical Engineering and Light Industry,Guangdong University of Technology,Guangzhou510006,China;Guangdong Provincial Key Laboratory of Emergency Test for Dangerous Chemicals,GuangdongInstitute of Analysis,Guangzhou510070,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第4期441-448,共8页
Journal of Instrumental Analysis
关键词
生物碱
高效液相色谱-串联质谱
精油类化妆品
alkaloids
high performance liquid chromatography-tandem mass spectrometry
essential oil cosmetics
