摘要
提出了超高效液相色谱-串联质谱法测定洗发水中西咪替丁、米诺地尔、美拉酮宁、香草酸甲酯、酮康唑、比马前列素、非那雄胺、塞替匹仑、尼鲁米特、氟罗地尔、螺内酯、氟他胺、拉坦前列素、度他雄胺等14种防脱育发类药物含量的方法.样品经水溶解、乙腈提取后,用氨基固相萃取柱净化.以 Waters Accquity UPLC BEH C18 色谱柱为固定相,以乙腈-含0.1%(体积分数)甲酸的2 mmol·L-1 乙酸铵溶液为流动相体系进行梯度洗脱;分离后的14种目标物经电喷雾离子源正、负离子模式扫描,多反应监测模式检测.结果表明:14种目标物的质量浓度在1.0～50.0 μg·L-1内与对应的峰面积呈线性关系,检出限(3S/N)为0.05～3.0 μg·kg-1;对空白样品进行3个浓度水平的加标回收试验,回收率为83.6%～99.0%,测定值的相对标准偏差(n=6)为5.6%～15%;方法用于10个洗发水样品分析,一个样品中检出米诺地尔、西咪替丁、塞替匹仑、酮康唑、尼鲁米特、氟罗地尔,另一个样品中检出美拉酮宁,检出量为0.4～47.8 μg·kg-1.
Abstract
A method for the determination of 14 anti-aging and hair growth drugs including cimetidine,minoxidil,melatonin,methyl vanillate,ketoconazole,bimatoprost,finasteride,setipiprant,nilutamide,fluridil,spironolactone,flutamide,latanoprost and dutasteride in shampoo by ultra-high performance liquid chromatography-tandem mass spectrometry was proposed.The sample was dissolved in water,extracted with acetonitrile,and purified with amino solid phase extraction column.Gradient elution was performed using Waters Accquity UPLC BEH C18 column as the stationary phase and acetonitrile-2 mmol·L-1 ammonium acetate solution containing 0.1%(volume fraction)formic acid as the mobile phase system.The 14 separated targets were scanned by electrospray ion source with positive and negative ion modes and detected by multi-reaction monitoring mode.It was shown that linear relationships between the mass concentrations and corresponding peak areas of 14 targets were kept in the range of 1.0-50.0 μg·L-1,with detection limits(3S/N)in the range of 0.05-3.0 μg·kg-1.Test for recovery was made on the blank sample at 3 concentration levels by standard addition method,giving results in the range of 83.6%-99.0%,and RSDs(n=6)of determined values ranged from 5.6%to 15%.The method was applied to the analysis of 10 shampoo samples.Minoxidil,cimetidine,setipiprant,ketoconazole,nilutamide and fluridil were detected in one sample,and melatonin was detected in another sample,with detection amounts in the range of 0.4-47.8 μg·kg-1.
NETL
NSTL
万方数据