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QuEChERS/高效液相色谱-串联质谱法测定面膜中10种荧光增白剂
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张虹艳,邱国玉,吴福祥,许晓辉,王小乔,朱天虹,李晨曦 兰州市食品药品检验所 
基金项目:甘肃省药品监督管理局青年科技创新项目(2019GSMPA008)
中文摘要:建立了QuEChERS/高效液相色谱-串联质谱法测定面膜中10种荧光增白剂的分析方法。样品经水溶解后,以乙腈提取目标化合物,加入NaCl和无水MgSO4,再通过C18填料和正丙基乙二胺(PSA)净化,离心氮吹浓缩,乙腈定容后上机检测。C18色谱柱分离,以10 mmol/L乙酸铵-乙腈梯度洗脱,多反应监测(MRM)正负离子模式交替扫描,外标法定量。结果显示,10种荧光增白剂在一定浓度范围内呈良好的线性,相关系数(r2)均大于0.99,正离子模式的6种目标化合物检出限(S/N=3)为0.05~1.0 μg/kg,定量下限为0.2~3.0 μg/kg,负离子模式的4种目标化合物检出限(S/N=3)为0.1~1.0 mg/kg,定量下限为0.3~2.0 mg/kg;方法平均回收率为64.4%~106%,相对标准偏差(n=6)为2.6%~8.5%,该方法操作简单,回收率高,适用于面膜中10种荧光增白剂的测定。
中文关键词:三重四极杆液质联用仪  荧光增白剂  面膜
 
Determination of White Agents in Facial Mask by QuEChERS/High Performance Liquid Chromatography-Tandem Mass Spectrometry
Abstract:A method based on QuEChERS coupled with high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) was developed for the determination of ten fluorescent white agents(FWAs) residues in facial mask.After mixed with water,the sample was extracted with acetonitrile,then added NaCl and MgSO4,cleaned up with C18 and primary secondary amine(PSA).The extracts were centrifuged,concentrated,and diluted with acetonitrile,then analyzed by HPLC-MS/MS.Separation of the FWAs was carried out on a C18 column with 10 mmol/L ammonium acetate and acetonitrile by gradient elution.The compounds were detected in positive/negative ion mode under multi reaction monitoring(MRM) mode.The quantitation was performed by exteral standard method.Results showed that there were good linear relationships for the FWAs in a certain concentration range with correlation coefficients(r2) greater than 0.99.In positive mode,the limits of detection(S/N=3) and the limits of quantitation(S/N=10) were in the ranges of 0.05-1.0 μg/kg and 0.2-3.0 μg/kg,respectively,while in negative mode,they both were 0.1-1.0 mg/kg and 0.3-2.0 mg/kg,respectively.The average recoveries for ten FWAs ranged from 64.4% to 106% with relative standard deviations(RSDs) of 2.6%-8.5%.With the advantages of simple operation and high recovery,the method is suitable for the determination of 10 FWAs in facial mask.
Key Words:high performance liquid chromatography-triple quadrupole mass spectrometry(HPLC-MS/MS)  fluorescent white agents(FWAs)  facial mask
引用本文:张虹艳,邱国玉,吴福祥,许晓辉,王小乔,朱天虹,李晨曦.QuEChERS/高效液相色谱-串联质谱法测定面膜中10种荧光增白剂[J].分析测试学报,2019,(9):1120-1125.
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