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超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速分析化妆品中17种喹诺酮类药物
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廖华勇,王景,李红玉 广州华鑫检测技术有限公司 
中文摘要:建立了一种水剂、乳液和非蜡基膏霜类化妆品中17种喹诺酮类药物的超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-Q Orbitrap HRMS)分析方法。样品采用0.1%甲酸(体积分数)乙腈混合溶液超声提取,正己烷液液萃取脱脂,经Agilent Poroshell EC C18(4.6 mm×150 mm,2.7 μm)色谱柱分离后,以全扫描/二级离子扫描(Full Scan/dd-MS2)进行定性筛查和定量检测,内标法定量。结果表明,17种喹诺酮类药物均在0.05~20.0 μg/L范围内呈良好的线性关系(r2>0.996 0),检出限和定量下限分别为0.5、1.0 μg/kg。在2、4、20 μg/kg 3个加标水平下,回收率为82.3%~108%,相对标准偏差(RSD,n=6)为3.5%~8.6%。该方法快速准确,灵敏度高,可用于化妆品中喹诺酮类药物的测定。
中文关键词:超高效液相色谱(UPLC)  高分辨质谱(HRMS)  化妆品  喹诺酮
 
Rapid Determination of 17 Quinolones in Cosmetics Using Ultra performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
Abstract:An ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry(UPLC-Q Orbitrap HRMS) was established for the determination of 17 quinolones in lotions,emulsions and non wax based cream cosmetics.The samples were ultrasonically extracted with 0.1%formic acid and acetonitrile mixed solvent,purified with n hexane,and then separated with an Agilent Poroshell EC C18(4.6 mm×150 mm,2.7 μm) column.The analytes were detected in Full Scan/dd-MS2 mode,and quantified by the internal standard method.Seventeen quinolones showed good linearities in the range of 0.05-200 μg/L with their correlation coefficients(r2) larger than 0.996 0.The limits of detection and quantitation for 17 quinolones were 0.5 μg/kg and 1.0 μg/kg,respectively.Average recoveries for 17 quinolones at three spiked levels of 2,4,20 μg/kg ranged from 82.3%to 108%with relative standard deviations(RSD,n=6) of 3.5%-8.6%.The method is rapid,accurate and sensitive,and is suitable for the determination of quinolone antibiotics in cosmetics.
Key Words:ultra performance liquid chromatography(UPLC)  high resolution mass spectrometry(HRMS)  cosmetics  quinolones
引用本文:廖华勇,王景,李红玉.超高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速分析化妆品中17种喹诺酮类药物[J].分析测试学报,2019,(9):1102-1107.
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