Application of Direct Analysis in Real Time-Electrostatic Field Orbitrap High Resolution Mass Spectrometry to Qualitative and Quantitative Analysis for 15 Anti-Allergics in Cosmetics
摘 要
提出了应用实时直接分析(DART)-静电场轨道阱高分辨质谱法对化妆品中15种抗过敏药物的定性和定量检测方法。称取样品0.50 g,加入50%(体积分数)乙醇溶液1.0 mL,于超声波水浴中超声处理5 min,涡旋振荡10 min后离心5 min,取上清液0.50 mL,加水0.5 mL混匀后再次离心5 min,取上清液,按仪器工作条件进行分析。采用Dip-it Samplers模式进样,进样量为1 μL。在正离子模式下,以一级全扫描-数据依赖性二级扫描(Full MS-ddMS2)进行定性分析,与自建二级(MS2)谱库进行比对,得到定性筛查结果;随即以平行反应监测(PRM)模式进行定量分析。所测的15种抗过敏药物的线性范围均在10 mg·L-1以内。由于所测得的15种药物的测定下限的信噪比远大于10倍,故本方法将测定下限定为0.5 mg·kg-1。用空白样品为基体,加入混合标准溶液进行回收试验,测得回收率在82%以上;测定值的相对标准偏差(n=6)均小于16%。应用本方法分析了20个市售化妆品样品,在其中的7个样品中检出苯海拉明,在1个样品中检出氯苯那敏,且所得结果与液相色谱-串联质谱法(LC-MS/MS)所测结果一致。
Abstract
The method of DART combined with electrostatic field orbitrap high resolution mass spectroscopy was applied to the qualitative and quantitative analysis of cosmetics for the 15 anti-allergics. 0.50 g of cosmetic sample was taken and ultrasonicated for 5 min with 1.0 mL of 50% (volume fraction) C2H5OH solution, and then shaken by swirling for 10 min, and centrifuged for 5 min. 0.50 mL of the supernatant was taken and mixed with 0.5 mL of water, centrifuged again for 5 min. The supernatant was taken and used for analysis under the instrumental working condition. Sample introduction with a volume of 1 μL was performed by the mode of Dip-it Samplers. Qualitative analysis was carried out by the mode of Full MS-ddMS2 under cationic mode. And by comparing with data of the self-established MS2 spectra database, sieved results of qualitative analysis were obtained. And then quantitative determinations were done under the PRM mode. Linearity ranges found for the 15 anti-allergics were same within 10 mg·L-1. Since values of lower limits of determination of the 15 drugs given by the S/N ratio were all much larger than 10, a value of 0.5 mg·kg-1 was set as the lower limit of determination for all the 15 drugs. Test for recovery was made by addition of the mixed standard solution to blank sample as matrix, giving results of recovery all over 82%; and values of RSDs (n=6) found were all less than 16%. 20 cosmetic samples obtained from the market were analyzed by the present method, benadryl was found in 7 of the 20 sample, and chlorpheniramine was found in one of the samples. Results found by this method were in consistency with those found by the LC-MS/MS.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202006011
所属栏目 工作简报
基金项目 原广东出入境检验检疫局科技计划项目(2018GDK14)
收稿日期 2019/10/16
修改稿日期
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作者单位点击查看
备注蓝草,工程师,硕士,主要从事仪器分析和食品化妆品检测工作
引用该论文: LAN Cao,SHAO Linzhi,XU Juan. Application of Direct Analysis in Real Time-Electrostatic Field Orbitrap High Resolution Mass Spectrometry to Qualitative and Quantitative Analysis for 15 Anti-Allergics in Cosmetics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(6): 686~691
蓝草,邵琳智,徐娟. 实时直接分析-静电场轨道阱高分辨质谱法应用于化妆品中15种抗过敏药物的定性和定量分析[J]. 理化检验-化学分册, 2020, 56(6): 686~691
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