超高效液相色谱法测定染发剂中的非那西丁  

Determination of phenacetin in hair dye by ultra-high performance liquid chromatography

作　　者：刘春生[1] 陈立伟[1] 吴玉銮[1] 罗海英[1] 冼燕萍[1] 王莉[1] 

机构地区：[1]广州市质量监督检测研究院国家化妆品质量监督检验中心(广州),广东广州510110

出　　处：《日用化学工业》2014年第1期50-53,共4页China Surfactant Detergent & Cosmetics

摘　　要：建立了一种测定染发剂中非那西丁的超高效液相色谱（UPLC）分析方法。染发剂样品经体积分数为70％的甲醇水溶液提取，再用正己烷进行反萃取后，采用BEHC18色谱柱，以乙腈-水为流动相进行梯度洗脱分离，结合保留时间和光谱图定性，以标准曲线定量。实验结果表明：非那西丁质量浓度在0．5—50．0mg·L^-1内与峰面积线性关系良好，相关系数大于0．9993；方法检出限（SIN=3）为3．0mg·kg^-1；加标量为10，20和50mg·kg^-1时，平均回收率为85．6％～97．9％，相对标准偏差（RSD，n=6）为3．7％～5．3％。An analysis method was established to determine phenacetin in hair dye by ultra - high performance liquid chromatography with a diode array detector （ UPLC - PDA）. The hair dye sample was extracted with 70% （volume fraction） methanol -water solution, reverse extracted with n -hexane, and analyzed by UPLC - PDA on a BEH Cls column,with acetonitrile-water as the mobile phase in gradient elution mode. The targets were qualitatively determined by retention time, confirmed by the ultraviolet spectrum, and quantified by standard graph. Test results indicated that in the phenaeetin mass concentration range of 0. 5 -50.0 mg ·L^-1the content shows a good linearity with the peak value with correlation coefficient （r） higher than 0. 999 3. The detection limit of phenacetin is 3.0 mg·kg^-1. When the spiking level is 10,20 and 50 mg ·kg^-1 ,the spiked recoveries of phenacetin are ranged within 85.6% and 97. 5.3% （n=6）. 9% ,and the precision （RSD） ranges from 3.7% to

关 键 词：染发剂 超高效液相色谱法 非那西丁 

分 类 号：O657.72[理学—分析化学] TQ658.34[理学—化学]