Determination of 9 Benzophenones for Ultraviolet Absorber in Cosmetics by High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘 要
建立了高效液相色谱-串联质谱法(HPLC-MS/MS)同时测定化妆品中9种二苯甲酮类紫外吸收剂含量的方法。将样品0.1 g用乙腈30 mL超声提取30 min,冷却至室温,稀释至50 mL,过滤,以C18色谱柱为固定相,以不同体积比的乙腈和0.1%(体积分数)甲酸溶液的混合液为流动相进行梯度洗脱。质谱分析中采用电喷雾正离子源和多反应监测模式检测,外标法定量。结果表明:样品基质效应较小,可不予考虑。9种二苯甲酮类化合物的质量浓度均在0.50~500 μg·L-1内与其对应的响应值呈线性关系,检出限(3s/k)为0.022~0.652 μg·L-1。连续测定混合标准溶液,9种二苯甲酮类紫外吸收剂测定值的相对标准偏差(n=6)均小于5.0%。按标准加入法进行回收试验,测得回收率为70.9%~116%。按此方法分析了15批样品,2批检出二苯酮-3,检出量为1.53%和4.67%,1批检出二苯酮-10,检出量为0.001 26%。
Abstract
The method for simultaneous determination of the 9 benzophenones for ultraviolet absorber in cosmetics by high performance liquid chromatography-tandem mass spectrometry was established. The sample (0.1 g) was treated in 30 mL of acetonitrile by ultrasonic extraction for 30 min, cooled to room temperature, diluted to 50 mL and filtered. C18 chromatographic column was used as the stationary phase, and a mixture of acetonitrile and 0.1% (φ) formic acid aqueous solution at different volume ratios was used as the mobile phase for gradient elution. The electrospray ionization source (ESI+) and multiple reaction monitoring mode were adopted into mass spectrometry analysis, and external standard method was used for quantitative analysis. It was showed that the matrix effect of the sample was small and could be ignored. Linear relationships between mass concentrations of the 9 benzophenones and their response values were kept in the same range of 0.50-500 μg·L-1, with detection limits (3s/k) in the range of 0.022-0.652 μg·L-1. The mixed standard solution were determined, with RSDs (n=6) of the determined values less than 5.0%. Test for recovery was made by standard addition method, giving values of recovery in the range of 70.9%-116%. 15 batches of samples were analyzed by this method, and benzophenone-3 was detected in 2 batches, with the detection amounts of 1.53% and 4.67%, and benzophenone-10 was detected in 1 batch, with the detection amount of 0.001 26%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202112008
所属栏目 工作简报
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收稿日期 2021/1/1
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备注鲁素雅,主管药师,硕士,主要从事药物分析研究
引用该论文: LU Suya,XING Haiyan,LIU Yang,WU Yichun,JIN Peng,CHEN Changyi. Determination of 9 Benzophenones for Ultraviolet Absorber in Cosmetics by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(12): 1104~1109
鲁素雅,邢海艳,刘洋,吴义春,金鹏,陈长毅. 高效液相色谱-串联质谱法测定化妆品中9种二苯甲酮类紫外吸收剂的含量[J]. 理化检验-化学分册, 2021, 57(12): 1104~1109
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【15】何乔桑,徐娜,李晶,等.高效液相色谱法测定化妆品中的12种紫外吸收剂[J].色谱, 2011,29(8):762-767.
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