Determination of 4 Benzotriazole Ultraviolet Absorbents in Cosmetics by Gas Chromatography
摘 要
提出了气相色谱法同时测定化妆品中甲酚曲唑(UV-P)、布美三唑(UV-326)、奥克三唑(UV-329)、甲酚曲唑三硅氧烷(DTTSO)等4种苯并三唑类紫外线吸收剂含量的方法。取样品0.300 0 g置于10 mL比色管中,用体积比1∶2的甲醇-四氢呋喃混合液稀释至刻度。若样品为水状化妆品,则超声提取10 min;若样品为乳液状、霜状和蜡状化妆品,则涡旋振荡5 min,超声提取10 min,离心2 min,取上层清液。得到的上述溶液经0.45 μm有机滤膜过滤后,加入1 mL 4.00 g·L-1内标(邻苯二甲酸二正辛酯)溶液,用乙醇定容至10 mL。采用HP-50+型石英毛细管色谱柱和氢火焰离子化检测器按照柱升温程序对溶液中4种苯并三唑类紫外线吸收剂进行分离,内标法定量。结果表明,UV-P、UV-326、UV-329和DTTSO与内标的质量比在一定范围内与峰面积比呈线性关系,检出限分别为23.64,12.03,39.88,57.46 mg·L-1。按照标准加入法进行回收试验,回收率为90.6%~103%,测定值的相对标准偏差(n=6)小于5.0%。方法用于分析12份不同基质化妆品,仅在2份乳液状化妆品中检出了UV-326和UV-329,检出量分别为9.56 mg·g-1和5.48 mg·g-1。
Abstract
A method for simultaneous determination of four benzotriazole ultraviolet absorbents including drometrizole (UV-P), bumetrizole (UV-326), octrizole (UV-329) and drometrizole trisiloxane (DTTSO) in cosmetics by gas chromatography was proposed. The sample (0.300 0 g) was placed in a 10 mL colorimetric tube and diluted to a scale with a mixture of methanol and tetrahydrofuran at a volume ratio of 1:2. For water-like cosmetics, the filtrate was obtained after ultrasonic extraction for 10 min. For emulsion, frost and waxy cosmetics, after vortex oscillation for 5 min, ultrasonic extraction for 10 min, and centrifugation for 2 min, the supernatant was taken. The above solution was passed through 0.45 μm organic filter membrane, and 1 mL of 4.00 g·L-1 internal standard (DNOP) solution was added. The mixture was made its volume up to 10 mL with ethanol. Four benzotriazole ultraviolet absorbents in the above solution were separated by HP-50+ quartz capillary column and flame ionization detector according to column temperature program, and quantitative analysis was carried out by the internal standard method. As shown by the results, linear relationships between peak area ratios and mass ratios of UV-P, UV-326, UV-329 and DTTSO to internal standard were found in definite ranges, with detection limits of 23.64, 12.03, 39.88, 57.46 mg·L-1, respectively. Test for recovery was made by the standard addition method, giving the results in the range of 90.6%-103%, with RSDs (n=6) of the determined values less than 5.0%. This method was applied to analysis of 12 cosmetics with different matrices, only UV-326 and UV-329 were detected in 2 emulsion cosmetics, with the detection amounts of 9.56 mg·g-1 and 5.48 mg·g-1.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202312012
所属栏目 工作简报
基金项目 安徽省教育厅自然科学研究重点项目(KJ2021A1406);安徽省高校优秀青年骨干教师国内访问研修项目(gxgnfx2021201);安徽省职业与成人教育学会重点项目(Azcj2021041);滁州职业技术学院校级重点科研项目(YJZ-2020-03)
收稿日期 2022/2/28
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备注王磊,副教授,研究方向为精细化学品的合成及色谱分析,stone@vip.qq.com
引用该论文: WANG Lei,JIANG Jie. Determination of 4 Benzotriazole Ultraviolet Absorbents in Cosmetics by Gas Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(12): 1437~1442
王磊,江洁. 气相色谱法测定化妆品中4种苯并三唑类紫外线吸收剂的含量[J]. 理化检验-化学分册, 2023, 59(12): 1437~1442
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【8】毛希琴,边海涛,曲宝成.高效液相色谱法测定化妆品中17种紫外线吸收剂[J].色谱, 2013,31(8):775-780.
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