潘秀丽, 邵长春, 李赟, 许晓辉, 王小乔, 张虹艳. QuEChERS-高效液相色谱/三重四极杆质谱联用法测定化妆品中防晒剂的检测方法[J]. 分析测试技术与仪器, 2023, 29(4): 384-391. DOI: 10.16495/j.1006-3757.2023.04.007
引用本文: 潘秀丽, 邵长春, 李赟, 许晓辉, 王小乔, 张虹艳. QuEChERS-高效液相色谱/三重四极杆质谱联用法测定化妆品中防晒剂的检测方法[J]. 分析测试技术与仪器, 2023, 29(4): 384-391. DOI: 10.16495/j.1006-3757.2023.04.007
PAN Xiuli, SHAO Changchun, LI Yun, XU Xiaohui, WANG Xiaoqiao, ZHANG Hongyan. Determination of Sunscreens in Cosmetics by QuEChERS-High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(4): 384-391. DOI: 10.16495/j.1006-3757.2023.04.007
Citation: PAN Xiuli, SHAO Changchun, LI Yun, XU Xiaohui, WANG Xiaoqiao, ZHANG Hongyan. Determination of Sunscreens in Cosmetics by QuEChERS-High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry[J]. Analysis and Testing Technology and Instruments, 2023, 29(4): 384-391. DOI: 10.16495/j.1006-3757.2023.04.007

QuEChERS-高效液相色谱/三重四极杆质谱联用法测定化妆品中防晒剂的检测方法

Determination of Sunscreens in Cosmetics by QuEChERS-High Performance Liquid Chromatography/Triple Quadrupole Mass Spectrometry

  • 摘要: 建立了防晒类化妆品中常用15种防晒剂的高效液相色谱/三重四极杆质谱联用分析方法和样品前处理方法. 样品中加入1 mL无水乙醇,用乙腈︰水(体积比4∶1)定容,超声提取后,QuEChERS柱净化,0 ℃下10000 r/min离心10 min,以含0.1%甲酸的乙腈溶液-含0.1%甲酸的2 mmol/L乙酸铵溶液为流动相,梯度洗脱,C18(2.1 mm×50 mm, 1.8 μm)色谱柱分离,多反应监测(MRM)正离子模式扫描,外标法定量. 结果显示:15种防晒剂在一定浓度范围内呈良好线性关系,相关系数均大于0.99,方法检出限为10~50 μg/kg. 方法平均回收率为68.4%~84.2%. 相对标准偏差(RSD)为1.7%~9.0%. 方法可用于防晒剂的检测,灵敏度高,重现性好,具有良好适应性.

     

    Abstract: The high performance liquid chromatography (HPLC) /triple quadrupole mass spectrometry method for analysis and sample pretreatment of 15 sunscreens commonly in sunscreen cosmetics was established. 1 mL of anhydrous ethanol was added to the sample, and the volume of the sample was fixed with acetonitrile∶water (volume ratio: 4∶1). After ultrasonic extraction, the sample was purified by a QuEChERS column, centrifuged at 0 ℃ for 10 min at 10 000 r/min. The sample was used as mobile phase with acetonitrile solution cotaining 0.1% formic acid-2 mmol/L ammonium acetate solution containing 0.1% formic acid, and then gradient elution was performed. The separation was carried out on a C18 (2.1 mm × 50 mm, 1.8 µm) column, scanned in positive ion mode with multiple reaction monitoring (MRM) and quantified by external standard method. The results showed that the 15 sunscreens showed good linearity in a certain concentration range, and the correlation coefficient was greater than 0.99. The detection limits of the method were 10~50 μg/kg. The average recoveries were 68.4%~84.2%, and the relative standard deviations (RSD) were 1.7%~9.0%. The method has a high sensitivity, good reproducibility and good adaptability for the detection of sunscreens.

     

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