摘要
目的通过优化提取条件、净化条件、仪器条件等参数,建立一种同时测定3种化妆品基质中20种生物碱的高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)分析方法。方法样品经含1%甲酸的乙腈-水(7∶3,V/V)混合溶剂超声提取,Qu ECh ERS技术净化,经Waters XBrige^(TM)C_(18)液相色谱柱分离后,在电喷雾离子源(electric spray ion source,ESI)正离子模式下通过多反应监测(multi-reaction monitoring,MRM)方式检测,外标法定量。结果20种生物碱在3种化妆品基质中具有良好的线性关系(r>0.996),方法的检出限为0.015~1.500μg/kg,定量限为0.049~4.900μg/kg,20种生物碱平均回收率为64.0%~122.0%,相对标准偏差为0.8%~13.3%。结论所建立的方法简便易操作、灵敏度高、重复性好、定量精准,适用于化妆品中多种生物碱的检测和安全性评价。
Objective By optimizing extraction conditions,purification conditions and instrument conditions,to establish a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method for the simultaneous determination of 20 alkaloids in three cosmetic substrates.Methods The sample was extracted by ultrasonic with acetonitrile-water(7∶3,V/V)mixed solvent containing 1%formic acid,purified by QuEChERS technology,separated by Waters XBrige^(TM) C_(18) liquid chromatography column,detected by multiple reaction monitoring(MRM)in positive mode of electric spray ion source(ESI),and quantified by external standard method.Results The 20 alkaloids had a good linear relationship in the three cosmetics substrates(r>0.996).The limits of detection and quantitation were 0.015-1.500μg/kg and 0.049-4.900μg/kg respectively.The average recoveries of 20 alkaloids were 64.0%-122.0%,and the relative standard deviations were 0.8%-13.3%.Conclusion The method is simple and easy to operate,with high sensitivity,good repeatability and accurate quantification,and is suitable for the detection and safety evaluation of various alkaloids in cosmetics.
作者
朱猛
赖淼菊
徐斯琦
熊艳蓝
崔淑丹
李强
ZHU Meng;LAI Miaoju;XU Siqi;XIONG Yanlan;CUI Shudan;LI Qiang(Physical and Chemical Department,Shanghai Putuo District Center for Disease Control and Prevention,Shanghai 200333,China)
出处
《职业与健康》
CAS
2024年第17期2346-2351,共6页
Occupation and Health
基金
上海市普陀区公共卫生青年课题(ptgw202107)
上海市普陀区公共卫生重点学科-卫生理化检验学(ptgw202001)。
关键词
化妆品
生物碱
高效液相色谱-串联质谱
QUECHERS
超声波提取
Cosmetics
Alkaloids
High performance liquid chromatography-tandem mass spectrometry
QuEChERS
Ultrasonic extraction
