超高效液相色谱法同时测定化妆品中的19种喹诺酮类抗生素  

Determination of 19 Quinolone Antibiotics in Cosmetics by Ultra Performance Liquid Chromatography

作　　者：陈静[1] 郑荣[1] 季申[1] 王柯[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《分析化学》2013年第6期931-935,共5页Chinese Journal of Analytical Chemistry

摘　　要：建立了同时测定化妆品中氧氟沙星、诺氟沙星、环丙沙星、双氟沙星、沙拉沙星、恶喹酸、氟甲喹等19种喹诺酮类抗生素的超高效液相分析方法。不同形态的化妆品样品经溶剂超声提取,提取液经高速离心处理,上清液以正己烷除脂,经0.22#m微孔滤膜过滤后取续滤液,采用Waters ACQUITY UPLC BEH ShieldRP C18反相色谱柱(100 mm×2.1 mm,1.7#m),以甲醇-乙腈(85∶15,V/V)-0.05 mol/L磷酸盐溶液(pH=3.6)梯度洗脱,然后采用二极管阵列检测器测定。本方法的相对标准偏差为0.4%～1.1%;回收率为75.5%～105.1%;各种喹诺酮类抗生素在5～100 mg/L的浓度范围内呈良好线性关系,相关系数均大于0.996;19种喹诺酮类抗生素的方法检出限为1.2～14.7 mg/kg。与传统的液相色谱法相比,本方法具有分离效率高、分析时间短、分析成分多等特点,已成功用于实际样品的检测。An ultra-liquid chromatographic（UPLC） method has been developed for the simultaneous determination of 19 quinolone antibiotics in cosmetics,ofloxacin,norfloxacin,ciproxacin,bifloxacin,sarafloxacin,oxolinic acid and flumequin etc.Different forms of cosmetic samples were prepared by ultrasonic extraction.The extraction solutions were obtained by high-speed centrifugation,the supernatant was degreased by hexane,and then was filtered by 0.22 μm millipore filter,and the continued filtrate was taken for analysis.A Waters reversed phase column,ACQUITY UPLC BEH Shield RP C18（100 mm×2.1 mm,1.7μm） was used with methanol ： acetonitrile（85 ∶ 15,V/V）-0.05 mol/L phosphate buffer（pH=3.6） as the mobile phase under the condition of gradient elution.And the diode array detector was used for the determination.The relative standard deviations（RSD） were 0.4%-1.1%;recoveries were 75.5%-105.1%;a variety of quinolones showed good linearity within the concentration range of 5-100 mg/L,correlation coefficients were greater than 0.996;detection limits were 1.2-14.7 mg/kg.This method has been successfully used for the determination of quinolone antibiotic in cosmetics products.

关 键 词：超高效液相色谱法 喹诺酮类抗生素 化妆品 

分 类 号：TQ658[化学工程—精细化工] O657.72[理学—分析化学]