摘要
目的建立HPLC-MS/MS定量测定化妆品中14种荧光增白剂的分析方法。方法样品经N,N-二甲基甲酰胺超声提取,选用Waters ACQUITY UPLC?BEH C_(18)(2.1 mm×50 mm,1.7μm)色谱柱,以甲醇-0.1%氨水水溶液梯度洗脱,流速0.3 mL·min^(–1),柱温40℃;质谱法采用三重四级杆质谱,电喷雾离子源,在正/负离子、多反应监测模式下进行扫描。结果14种荧光增白剂在定量范围内线性关系良好,相关系数均>0.99,定量限为0.01~20μg·g^(–1),检出限为0.004~8μg·g^(–1);在3个添加水平下的平均回收率为85.4%~108.9%,相对标准偏差为0.3%~7.2%。结论该方法灵敏度高,专属性强,操作简单方便,适用于化妆品中14种荧光增白剂的含量测定。
OBJECTIVE To establish a method for the determination of fourteen fluorescent whitening agents in cosmetics by HPLC-MS/MS.METHODS Samples were extracted on a Waters ACQUITY UPLC?BEH C_(18)(2.1 mm×50 mm,1.7μm) column after ultrasonic extracted by DMF with the mobile phase consisted of methanol-0.1%ammonia water solution by gradient elution.The flow rate was 0.3 mL·min^(–1).The column temperature was 40℃.MS was performed using triple quadrupole mass spectrometry.Electrospray ionization source was operated in the positive/negative mode using multiple reaction monitoring scanning mode.RESULTS The results showed that there were good linear relationships for the fluorescent whitening agents in a certain concentration range with correlation coefficients(r) greater than 0.99.The limits of quantification were 0.01-20μg·g^(–1) and the limits of detection were 0.004-8μg·g^(–1).The average recoveries at three spiked levels were in the range of 85.4%-108.9%,and the relative standard deviation were in the range of 0.3%-7.2%.CONCLUSION The method has high sensitivity,strong specificity,simple and convenient operation,and is suitable for the detection of fourteen fluorescent whitening agents in cosmetics.
作者
汪霞
林丽琴
杨直
高丽琼
王秀秀
金朦娜
陈鸿健
WANG Xia;LIN Liqin;YANG Zhi;GAO Liqiong;WANG Xiuxiu;JIN Mengna;CHEN Hongjian(Hangzhou Institute for Food and Drug Control,Hangzhou 310022,China)
出处
《中国现代应用药学》
CAS
CSCD
北大核心
2023年第23期3236-3244,共9页
Chinese Journal of Modern Applied Pharmacy
基金
浙江省药品监管系统科技计划项目(2021026)。
