高效液相色谱-电感耦合等离子体质谱法同时测定化妆品中5种含溴防腐剂
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摘要
建立了同时测定化妆品中苯扎溴铵、2-溴-2-硝基-1,3-丙二醇、5-溴-5-硝基-1,3-二■烷、甲基二溴戊二腈、溴氯芬5种含溴防腐剂的高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)。样品经含0.1%甲酸的甲醇溶液超声提取后,采用Agilent Eclipse-C_(18)(150 mm×4.6 mm,5μm)色谱柱分离,以0.1%甲酸-甲醇为流动相进行梯度洗脱,ICP-MS测定组分中的~(79)Br,以保留时间定性,外标法定量。5种含溴防腐剂均在0.5～100 mg/L范围内线性关系良好(r>0.999),检出限为1.5～3.0μg/g,不同基质化妆品中的回收率为91.2%～108%,相对标准偏差(n=6)为1.3%～4.2%。该方法快速、准确、灵敏、专属性强,适用于化妆品中5种含溴防腐剂的定性定量分析。
A novel high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS) was established for the determination of five bromine contained preservatives,i.e.benzalkonium bromide,2-bromo-2-nitro-1,3-propanediol,5-bromo-5-nitro-1,3-dioxane,methyldibromo glutaronitrile and bromochlorophene in cosmetics.The samples were ultrasonically pretreated with methanol containing 0.1%formic acid.The analytes containing ~(79)Br were separated on an Agilent Eclipse-C_(18) column(150 mm×4.6 mm,5 μm) using 0.1%formic acid-methanol as mobile phases by gradient elution,and then analyzed by ICP-MS with external standard method.There were good linear relationships for five analytes in the range of 0.5-100 mg/L with correlation coefficients(r) larger than 0.999.The detection limits for five bromine contained preservatives were in range of 1.5-3.0 μg/g.Recoveries for the analytes in different spiked cosmetics matrixes ranged from 91.2%to 108%with relative standard deviations(n=6) of 1.3%-4.2%.The method was fast,accurate,sensitive and selective,and was suitable for the simultaneous determination of five bromine contained preservatives in cosmetics.
A novel high performance liquid chromatography-inductively coupled plasma mass spectrometry(HPLC-ICP-MS) was established for the determination of five bromine contained preservatives,i.e.benzalkonium bromide,2-bromo-2-nitro-1,3-propanediol,5-bromo-5-nitro-1,3-dioxane,methyldibromo glutaronitrile and bromochlorophene in cosmetics.The samples were ultrasonically pretreated with methanol containing 0.1%formic acid.The analytes containing ~(79)Br were separated on an Agilent Eclipse-C_(18) column(150 mm×4.6 mm,5 μm) using 0.1%formic acid-methanol as mobile phases by gradient elution,and then analyzed by ICP-MS with external standard method.There were good linear relationships for five analytes in the range of 0.5-100 mg/L with correlation coefficients(r) larger than 0.999.The detection limits for five bromine contained preservatives were in range of 1.5-3.0 μg/g.Recoveries for the analytes in different spiked cosmetics matrixes ranged from 91.2%to 108%with relative standard deviations(n=6) of 1.3%-4.2%.The method was fast,accurate,sensitive and selective,and was suitable for the simultaneous determination of five bromine contained preservatives in cosmetics.
引文
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