GC-MS/MS Determination of 12 UV Absorbers in Sunscreening Cosmetics
摘 要
称取防晒化妆品样品5.0 g,加入饱和氯化钠溶液1 mL,充分混匀后用二氯甲烷为溶剂先后2次萃取样品中12种紫外线吸收剂(UVA)。每次萃取用二氯甲烷5 mL,涡旋振荡60 s,超声萃取30 min,并高速离心5 min。收集并合并2次萃取的上清液,吹氮蒸发至近干,用二氯甲烷溶解残渣并定容至1.0 mL。采用DB-5MS色谱柱为分离柱,进样量为1 μL,在80~300℃区间采用程序升温模式可在30 min内对所测12种UVA实现分离;在电子轰击离子源和选择反应监测模式条件下进行串联质谱测定。测得12种UVA的线性范围均在0.01~1.0 mg·L-1之间,检出限(3S/N)在1.0~3.0 μg·kg-1之间。在不含目标物的空白防晒化妆品中加入12种UVA的混合标准溶液后,按方法分析求得其回收率及测定值的相对标准偏差(n=6),测得两者的结果依次在93.0%~100%之间和1.2%~4.1%之间。
Abstract
A portion (5.0 g) of the sunscreening cosmetic sample was mixed thoroughly with 1 mL of saturated NaCl solution and extracted twice with CH2Cl2 (5 mL for each extraction) to transfer 12 UV absorbers (UVA) into the organic solvent by swirling for 60 s, extracting ultrasonically for 30 min and centrifuging for 5 min with high speed. The supernatants from the 2 extractions were combined and evaporated to near dryness by N2-blowing. The residue was dissolved and made its total volume to 1.0 mL with CH2Cl2. An aliquot of 1 μL of the CH2Cl2 solution was introduced to the chromatographic column of DB-5MS for separation of the 12 UVA under the mode of programed temperature elevation in the temperature interval from 80℃ to 300℃. A clear-cut separation of the 12 UVA was fulfilled within 30 min and their determination was carried out by MS/MS under the modes of EI-ionization source and selected reaction monitoring. Linearity ranges for the 12 UVAs were found same between 0.01-1.0 mg·L-1. Values of their detection limits (3S/N) found were in the range of 1.0 to 3.0 μg·kg-1. Test for recovery and precision was performed by addition of mixed standard solution of the 12 UVA to a blank sunscreening cosmetic sample, giving results of recovery in the range from 93.0% to 100%, and results of RSDs (n=6) in the range from 1.2% to 4.1%.
中图分类号 O652.63 DOI 10.11973/lhjy-hx201909005
所属栏目 工作简报
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收稿日期 2019/1/4
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备注周宝龙,讲师,硕士,研究方向为工业分析检验,3381226538@qq.com
引用该论文: ZHOU Baolong. GC-MS/MS Determination of 12 UV Absorbers in Sunscreening Cosmetics[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2019, 55(9): 1013~1018
周宝龙. 气相色谱-串联质谱法测定防晒化妆品中12种紫外线吸收剂[J]. 理化检验-化学分册, 2019, 55(9): 1013~1018
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参考文献
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【3】高立雪,张卫强,喻晓毅.防晒化妆品中的防晒剂使用频度分析[J].现代预防医学, 2011,38(7):1324-1325.
【4】CAI H, SHEN D, YUAN L, et al. Developing thermally resistant polydopamine@nano turbostratic BN@CeO2 double core-shell ultraviolet absorber with low light-catalysis activity and its grafted high performance aramid fibers[J]. Applied Surface Science, 2018,452:389-399.
【5】HEO S, HWANG H S, JEONG Y, et al. Skin protection efficacy from UV irradiation and skin penetration property of polysaccharide-benzophenone conjugates as a sunscreen agent[J]. Carbohydrate Polymers, 2018,195:534-541.
【6】龙飞,卢平,任璐,等.二苯甲酮类紫外吸收剂人体暴露的研究进展[J].环境与健康杂志, 2015,32(7):643-646.
【7】高礼,袁涛,王文华.水环境中有机紫外防晒剂的生态风险评价[J].环境与健康杂志, 2015,32(4):332-336.
【8】LAZOVICH D, VOGEL R I, BERWICK M, et al. Melanoma risk in relation to use of sunscreen or other sun protection methods[J]. Cancer Epidemiology Biomarkers & Prevention, 2011,20(12):2583-2593.
【9】杨铭,胡丹,王晨蕾.气相色谱法同时测定防晒类化妆品中13种紫外吸收剂[J].理化检验-化学分册, 2018,54(11):1324-1328.
【10】夏平,李勇.薄层色谱法测定化妆品中多种防晒剂[J].环境与健康杂志, 1997,10(5):227-228.
【11】王雪梅,王娟,杜彤彤,等.基于石墨烯海绵的固相萃取-液相色谱法测定化妆品中6种紫外吸收剂[J].色谱, 2018,36(3):190-194.
【12】虞成华,巢强国,曹程明,等.高效液相色谱法测定化妆品中防晒剂[J].理化检验-化学分册, 2010,46(11):1273-1278.
【13】崔凤杰,谷婕,张坤,等.高效液相色谱法测定化妆品中22种紫外吸收剂[J].日用化学工业, 2017,47(1):52-56.
【14】矫筱蔓,贾铭婧,庞燕军.化妆品中三种紫外吸收剂检测方法的建立[J].中国药师, 2017,20(5):949-952.
【15】林维宣,孙兴权,马杰.液相色谱-串联质谱法同时检测防晒化妆品中的11种紫外吸收剂[J].色谱, 2013,31(5):410-415.
【16】张强,刘艳,顾华,等.高效液相色谱法测定塑料食品包装材料中8种苯并三唑类紫外吸收剂[J].分析试验室, 2017,36(3):358-362.
【17】李英,王成云,刘丽,等.气相色谱-质谱法测定化妆品中的防晒剂[J].分析试验室, 2003,22(3):77-80.
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