摘要 建立了一种超高效液相色谱-二极管阵列检测法同时测定不同种类化妆品中22种防晒剂的方法。样品首先加入少量四氢呋喃,涡旋、分散、混匀(蜡质化妆品可于50℃超声,以便分散完全),然后加入0.1%(v/v)甲酸乙醇溶液振摇、超声提取,稀释、过滤后经Poroshell 120 EC-C18(100 mm×4.6 mm,2.7μm)分离,乙腈-异丙醇-50 mmol/L乙酸铵水溶液(含0.05%(v/v)甲酸)梯度洗脱,二极管阵列检测器检测,检测波长311 nm,外标法定量。结果表明,22种防晒剂在各自的范围内线性关系良好,相关系数(r)均在0.998以上。选取两种不同基质类型的样品,在低、中、高3个不同添加水平下的平均回收率为85.2%~112.3%,相对标准偏差(RSD)在0.5%~6.5%之间,方法的检出限和定量限分别为0.7~64 mg/kg和2.4~215 mg/kg。在2、10、50 mg/L3个水平的混合标准溶液的稳定性试验中,甲酚曲唑三硅氧烷组分12 h内稳定,其余组分36 h内稳定。采用该方法测定市售16份化妆品中的防晒剂,其中5份样品检测结果与厂家提供的配方值匹配良好。与《化妆品安全技术规范》(2015年版)收载方法相比,该方法在流动相组成和提取溶剂选择方面,摒弃了四氢呋喃和高氯酸等腐蚀性溶剂的使用,改善了弱极性组分的提取效率,同时增加了检测组分二苯酮-2,被测物稳定性更好,实验操作更便利高效,分离效果更好,结果更准确,兼顾绿色环保,可用于化妆品防晒剂的日常检测。 A fast and simple ultra-high-performance liquid chromatography using diode array detector(UHPLC-DAD)technique has been developed for the simultaneous determination of 22 sunscreen agents(UV filters),viz.phenylbenzimidazole sulfonic acid(PBS),terephthalydene dicamphor sulfonic acid(TDS),benzophenone-4(BZ4),camphor benzalkonium methosulfate(CBM),benzophenone-2(BZ2),benzylidene camphor sulfonic acid(BCS),benzophenone-3(BZ3),3-benzylidene camphor(3BC),isoamyl p-methoxycinnamate(IMC),4-methylbenzylidene camphor(MBC),diethylamino hydroxybenzoyl hexyl benzoate(DHHB),octocrylene(OCR),butyl methoxydibenzoyl methane(BDM),ethylhexyl dimethyl PABA(EDP),ethylhexyl methoxycinnamate(EMC),homosalate(HS),ethylhexyl salicylate(ES),diethylhexyl butamido triazone(DBT),ethylhexyl triazone(ET),drometrizole trisiloxane(DRT),methylene bis-benzotriazolyl tetramethylbutylphenol(MBP),and bis-ethylhexyloxyphenol methoxyphenyl triazine(EMT)in cosmetic products.Different parameters,such as column type,oven temperature,mobile phase composition,and detection wavelength,were studied.The best chromatographic separation was obtained under the following conditions:Poroshell 120 EC-C18(100 mm×4.6 mm,2.7μm)column set at 25℃and gradient acetonitrile-isopropanol-water(containing 50 mmol/L ammonium acetate and 0.05%(v/v)formic acid)as the mobile phase,pumped at a flow rate of 0.5 mL/min,with a wavelength of 311 nm.The proposed UHPLC-DAD technique provided separation of the 22 target sunscreen agents within 35 min,with the optimized sample pretreatment procedure below.First,samples were mixed thoroughly by adding 2 mL or 5 mL tetrahydrofuran,followed by vortex and dispersal.If the wax samples were still not homogenized completely,an ultrasonic dispersal protocol with heating to 50℃was adopted.Second,the homogeneous samples were ultrasonically extracted with ethanol containing 0.1%(v/v)formic acid.The developed method showed good linear relationships,with correlation coefficients of no less than 0.998.Two kinds of samples with different matrix types
出处 《色谱》 CAS CSCD 北大核心 2021年第4期415-423,共9页 Chinese Journal of Chromatography
基金 广西药品监督管理局科研计划(2019-06).
关键词 超高效液相色谱 防晒剂 紫外吸收剂 化妆品 ultra-high performance liquid chromatography(UHPLC) sunscreen agents ultraviolet(UV)filters cosmetics
分类号 O658 [理学—分析化学]
