HPLC-DAD法和GC-FID法测定化妆品中6-甲基香豆素的方法比较
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摘要
对化妆品中6-甲基香豆素测定的HPLC-DAD法和GC-FID法进行了比较,如有阳性样品,用GC-MS法进行确证。用甲醇提取化妆品中6-甲基香豆素,优化两种方法的色谱条件,并对样品进行测定,比较了两种方法的回收率、精密度、相关系数、检出限及定量限。结果表明,两种测定方法的线性关系良好,HPLC-DAD法加标回收率为92.20%~102.80%,RSD为0.77%~2.00%,检出限为0.05 mg/kg,定量限为0.17 mg/kg;GC-FID法加标回收率为97.30%~103.28%,RSD为0.47%~4.87%,检出限为1.3 mg/kg,定量限为5.0 mg/kg;HPLC-DAD法比GC-FID法的检出限更低且灵敏度更高,对含量低的样品更有优势。
To compare a high performance liquid chromatography with the diode array detector(HPLC-DAD)method and a gas chromatograph with the flame ionization detector(GC-FID) method for the determination of 6-methyl coumarin in cosmetics.Positive samples were confirmed by GC-MS.Methanol was used to extract6-methyl coumarin from cosmetics,and the chromatographic conditions of the two methods were optimized.Samples were measured and the recoveries,precisions,correlation coefficients,detection limits,and quantitative limits of the two methods were compared.Results show that both of the two methods have good linear relationships in the range of their respective mass concentration.The recoveries of HPLC-DAD is between 92.20% to 102.80%,the RSD is between 0.77% to 2.00%,the detection limit is 0.05 mg/kg and the quantitative limit is 0.17 mg/kg.The recoveries of GC-FID is between 97.30% to 103.28%,the RSD is between 0.47% to 4.87%,the detection limit is 1.3 mg/kg and the quantitative limit is 5.0 mg/kg.HPLC-DAD method has a lower detection limit and higher sensitivity than GC-FID method,and has more advantages in determining low-content samples.
To compare a high performance liquid chromatography with the diode array detector(HPLC-DAD)method and a gas chromatograph with the flame ionization detector(GC-FID) method for the determination of 6-methyl coumarin in cosmetics.Positive samples were confirmed by GC-MS.Methanol was used to extract6-methyl coumarin from cosmetics,and the chromatographic conditions of the two methods were optimized.Samples were measured and the recoveries,precisions,correlation coefficients,detection limits,and quantitative limits of the two methods were compared.Results show that both of the two methods have good linear relationships in the range of their respective mass concentration.The recoveries of HPLC-DAD is between 92.20% to 102.80%,the RSD is between 0.77% to 2.00%,the detection limit is 0.05 mg/kg and the quantitative limit is 0.17 mg/kg.The recoveries of GC-FID is between 97.30% to 103.28%,the RSD is between 0.47% to 4.87%,the detection limit is 1.3 mg/kg and the quantitative limit is 5.0 mg/kg.HPLC-DAD method has a lower detection limit and higher sensitivity than GC-FID method,and has more advantages in determining low-content samples.
引文
[1]Zhang Guangliu,Yang Ming,Xia Juanjuan,et al.Preparation and study of 6-methylcoumarin molecular imprinting polymer microspheres and copolymer microspheres[J].Journal of Wuhan Polytechnic University,2013,32(3):22-26.
[2]Li Jie,Wang Chao,Wu Ting,et al.Determination of three coumarin compounds in cosmetics by HPLC[J].China Surfactant Detergent&Cosmetics,2006,36(4):257-259.
[3]Tian Furao,Wang Xuqiang,Sun Wenshan.Determination of 6-methyl coumarin in cosmetics by HPLC-VWD[J].Flavour Fragrance Cosmetics,2012(1):30-32.
[4]Chen Wenjun,Tang Lei,Wu Meng.Simultaneous determination of benzoic acid and 6-methyl coumarin in cosmetics by high performance liquid chromatography[J].Guangzhou Chemical Industry,2013,41(3):100-101,111.
[5]Xiao Shangjia,Wang Shiping.Determination of 6-methyl coumarin in cosmetics by gas chromatography[J].Journal of Environment and Health,2002,19(2):146-147.
[6]Wang Xing,Cai Tianpei,Wang Chao,et al.Determination of safrole and 6-methyl coumarin in cosmetics using GC and GC-MS[J].Journal of Environment and Health,2007,24(5):358-359.
[7]Xu Kehua,Zhou Zhishen.Synthesis of 6-methyl coumarin[J].Shandong Chemical Industry,1997(1):14-17.
[2]Li Jie,Wang Chao,Wu Ting,et al.Determination of three coumarin compounds in cosmetics by HPLC[J].China Surfactant Detergent&Cosmetics,2006,36(4):257-259.
[3]Tian Furao,Wang Xuqiang,Sun Wenshan.Determination of 6-methyl coumarin in cosmetics by HPLC-VWD[J].Flavour Fragrance Cosmetics,2012(1):30-32.
[4]Chen Wenjun,Tang Lei,Wu Meng.Simultaneous determination of benzoic acid and 6-methyl coumarin in cosmetics by high performance liquid chromatography[J].Guangzhou Chemical Industry,2013,41(3):100-101,111.
[5]Xiao Shangjia,Wang Shiping.Determination of 6-methyl coumarin in cosmetics by gas chromatography[J].Journal of Environment and Health,2002,19(2):146-147.
[6]Wang Xing,Cai Tianpei,Wang Chao,et al.Determination of safrole and 6-methyl coumarin in cosmetics using GC and GC-MS[J].Journal of Environment and Health,2007,24(5):358-359.
[7]Xu Kehua,Zhou Zhishen.Synthesis of 6-methyl coumarin[J].Shandong Chemical Industry,1997(1):14-17.