高效液相色谱法同时测定化妆品中12种防腐剂
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摘要
采用高效液相色谱法同时检测化妆品中12种防腐剂的含量。C18色谱柱(250 mm×4.6 mm×5μm)为分析柱,甲醇+乙腈+0.02 mol·L-1磷酸二氢钠(pH=3.5)为流动相,梯度洗脱。2-溴-2-硝基丙烷-1,3-二醇和苯甲醇检测波长为210 nm;甲基氯异噻唑啉酮和甲基异噻唑啉酮检测波长为280 nm;其它组分检测波长为254 nm。结果表明各组分在浓度为4.242~299.0 mg/L范围内与目标峰面积均呈较好的线性关系,R均大于0.9999。加标回收率在92.6%~108%之间,各组分的相对标准偏差(n=7)在1.2%~3.1%之间。方法相对《化妆品卫生规范》相比,更简单、易操作、实用性更强,适用于化妆品中多种防腐剂的同时测定。
HPCL was developed for the determination of 12 preservatives in cosmetics. The sample was separated with a mixture of methanol, acetonitrile and 0.02 mol·L-1 Na H2 PO4 as mobile phase on a C18 column(250 mm×4.6 mm×5 μm) with gradient elution. The detection wavelength was 210 nm for 2-bromo-2-nitropropane-1,3-diol and benzyl alcohol, 280 nm for metylchloro isothiazolinone and methylisothiazolinone, and 254 nm for others. Good linear relationship between values of peak area and concentration of preservatives was obtained in the range from 4.242 to 299.0 mg/L, and the correlation coefficients were above 0.9999. The recovery rate ranged 92.6 % from 108 %, and relative standard deviations(RSD)(n=7) were between 1.2 % and 3.1 %. The method is simpler, easier to operate, more practical compared to Hygienic Standard for Cosmetics and can be applied to the determination of 12 preservatives in cosmetics simultaneously.
HPCL was developed for the determination of 12 preservatives in cosmetics. The sample was separated with a mixture of methanol, acetonitrile and 0.02 mol·L-1 Na H2 PO4 as mobile phase on a C18 column(250 mm×4.6 mm×5 μm) with gradient elution. The detection wavelength was 210 nm for 2-bromo-2-nitropropane-1,3-diol and benzyl alcohol, 280 nm for metylchloro isothiazolinone and methylisothiazolinone, and 254 nm for others. Good linear relationship between values of peak area and concentration of preservatives was obtained in the range from 4.242 to 299.0 mg/L, and the correlation coefficients were above 0.9999. The recovery rate ranged 92.6 % from 108 %, and relative standard deviations(RSD)(n=7) were between 1.2 % and 3.1 %. The method is simpler, easier to operate, more practical compared to Hygienic Standard for Cosmetics and can be applied to the determination of 12 preservatives in cosmetics simultaneously.
引文
[1]丁怡,张静.高效液相色谱法同时测定化妆品中7种抗生素和12种防腐剂[J].中国卫生检验杂志,2017,27(1):18-26.
[2]高立雪,胡俊明.防腐剂4-羟基苯甲酸酯类在化妆品中使用情况分析[J].环境卫生学杂志,2012,2(2):74-75.
[3]郑荣,茹歌,王柯.高效液相色谱-串联质谱法测定化妆品中16种防腐剂[J].中国卫生检验杂志,2016,26(19):2758-2761.
[4]蔡伦华,康晓熙,万莉,等.防腐剂4-羟基苯甲酸酯类在化妆品中使用现状分析[J].职业卫生与病伤,2016,31(3):177-179.
[5]曾铭,喻零春,尹君玲,等.高效液相色谱法测定化妆品中防腐剂[J].理化检验-化学分册,2012,48(10):1203-1205.
[6]Lucia SP,Gerardo AR,Lamas JP,et al.Analysis of multi-class preservatives in leave-on and rinse-off cosmetics by matrix solid-phase dispersion[J].Anal Bioanal Chem,2011,401(10):3293-3304.
[7]Liao CY,Liu F,Kannan K.Occurrence of and Dietary Exposure to Parabens in Foodstuffs from the United States[J].Environmental science&technology,2013,47(8):3918-3925.
[8]陆志芸,李勤,张辉,等.化妆品中防腐剂苯甲酸及其盐类和酯类的高效液相色谱法测定.香料香精化妆品,2011,2011(2):20-24.
[9]Borremans M,Loco JV,Roos P,et al.Validation of HPLC Analysis of2-Phenoxyethanol,1-Phenoxypropan-2-ol,Methyl,Ethyl,Propyl,Butyl and Benzyl 4-Hydroxybenzoate(Parabens)in Cosmetic Products,with Emphasis on Decision Limit and Detection Capability[J].Chromatographia,2004,59(1):47-53.
[10]符策奕,梁颖,许文佳,等.液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂[J].药物分析杂志,2016,36(8):1456-1464.
[11]Orton DI,Wilkinson JD.Cosmeticallergy:incidence,diagnosis,and management[J].Am J Clin Dermatol.2004,5(5):327-337.
[12]温玉鳞.药物与化学物质毒性数据[M].天津:天津科学技术出版社,1987.
[13]陈科,刘翠红,李练培.超高效液相色谱法测定化妆品中的6种防腐剂[J].广东化工,2016,17(43):189-191.
[14]严倩茹,邬伟魁.超高效液相色谱在化妆品禁用药物及限用物质和功效成分分析中的应用[J].中国药事,2017,31(1):74-78.
[15]化妆品卫生规范(2007年版)[S].
[16]化妆品卫生规范(2015年版)[S].
[2]高立雪,胡俊明.防腐剂4-羟基苯甲酸酯类在化妆品中使用情况分析[J].环境卫生学杂志,2012,2(2):74-75.
[3]郑荣,茹歌,王柯.高效液相色谱-串联质谱法测定化妆品中16种防腐剂[J].中国卫生检验杂志,2016,26(19):2758-2761.
[4]蔡伦华,康晓熙,万莉,等.防腐剂4-羟基苯甲酸酯类在化妆品中使用现状分析[J].职业卫生与病伤,2016,31(3):177-179.
[5]曾铭,喻零春,尹君玲,等.高效液相色谱法测定化妆品中防腐剂[J].理化检验-化学分册,2012,48(10):1203-1205.
[6]Lucia SP,Gerardo AR,Lamas JP,et al.Analysis of multi-class preservatives in leave-on and rinse-off cosmetics by matrix solid-phase dispersion[J].Anal Bioanal Chem,2011,401(10):3293-3304.
[7]Liao CY,Liu F,Kannan K.Occurrence of and Dietary Exposure to Parabens in Foodstuffs from the United States[J].Environmental science&technology,2013,47(8):3918-3925.
[8]陆志芸,李勤,张辉,等.化妆品中防腐剂苯甲酸及其盐类和酯类的高效液相色谱法测定.香料香精化妆品,2011,2011(2):20-24.
[9]Borremans M,Loco JV,Roos P,et al.Validation of HPLC Analysis of2-Phenoxyethanol,1-Phenoxypropan-2-ol,Methyl,Ethyl,Propyl,Butyl and Benzyl 4-Hydroxybenzoate(Parabens)in Cosmetic Products,with Emphasis on Decision Limit and Detection Capability[J].Chromatographia,2004,59(1):47-53.
[10]符策奕,梁颖,许文佳,等.液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂[J].药物分析杂志,2016,36(8):1456-1464.
[11]Orton DI,Wilkinson JD.Cosmeticallergy:incidence,diagnosis,and management[J].Am J Clin Dermatol.2004,5(5):327-337.
[12]温玉鳞.药物与化学物质毒性数据[M].天津:天津科学技术出版社,1987.
[13]陈科,刘翠红,李练培.超高效液相色谱法测定化妆品中的6种防腐剂[J].广东化工,2016,17(43):189-191.
[14]严倩茹,邬伟魁.超高效液相色谱在化妆品禁用药物及限用物质和功效成分分析中的应用[J].中国药事,2017,31(1):74-78.
[15]化妆品卫生规范(2007年版)[S].
[16]化妆品卫生规范(2015年版)[S].