摘要
建立超高效液相色谱-串联质谱(UPLC-MS/MS)法,同时测定祛痘类化妆品中磺胺吡啶、磺胺甲二唑、磺胺甲氧嗪、磺胺氯哒嗪等10种磺胺类药物的检测方法。样品经乙腈超声提取,冷冻离心后,上清液加水定容,采用Waters ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm)进行分离,以0.1%甲酸水溶液-乙腈(含0.1%甲酸)为流动相进行梯度洗脱,在电喷雾正离子模式下,以多反应监测(MRM)方式进行测定。结果表明,10种磺胺类药物在相应浓度范围内线性关系良好,相关系数(r)均大于0.995。方法检出限为1~10μg/kg,定量限为2~32μg/kg。样品的加标平均回收率为93.5%~110.9%,相对标准偏差为1.5%~5.7%。该方法具备操作简便快捷,灵敏度高等优点,可用于祛痘类化妆品中10种磺胺类药物的测定。
A method for the determination of 10 sulfonamides in Anti-Acne Cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The sample was extracted by ultrasonic extraction using acetonitrile,freezing centrifuged,diluted with water,then the analytes were separated on Waters ACQUITY UPLC HSS T3 column(100 mm×2.1 mm,1.8 μm) by gradient elution using 0.1% formic acid water solution and acetonitrile(0.1% formic acid) as the mobile phase.The electrospray ion source was operated in the positive ion mode using the multiple reaction monitoring method.The correlation coefficient of the linear calibration curves were greater than 0.995 in the corresponding mass concentration ranges,the average recoveries at three spiked levels ranged from 93.5% to 110.9%,the relative standard deviations of 1.5%-5.7%.The method was simple,rapid,accurate,and suitable for the detection of 10 sulfonamides in Anti-Acne Cosmetics.
作者
张丽蓉
谢宋阳
肖紫芬
卢端萍
陈硕
ZHANG Lirong;XIE Songyang;XIAO Zifen;LU Duanping;CHEN Shuo(Fujian Institute for Food and Drug Quality Control,Fuzhou 350001)
出处
《分析科学学报》
CAS
CSCD
北大核心
2021年第6期814-818,共5页
Journal of Analytical Science