固相萃取-气相色谱/质谱法测定化妆品中多种季铵盐化合物
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摘要
建立了快速测定化妆品中多种季铵盐类化合物的固相萃取-气相色谱/质谱法。以甲醇作为溶剂提取目标化合物,弱阳离子固相萃取柱净化,以D9十六烷基三甲基氯化铵做内标,采用电子轰击(EI)-选择离子模式(SIM)进行定性与定量分析同时测定化妆品中5种季铵盐化合物十二烷基三甲基氯化铵(DTAC)、十四烷基三甲基氯化铵(TTAC)、十六烷基三甲基溴化铵(CTAB)、十八烷基三甲基氯化铵(STAC)、二十二烷基三甲基氯化铵(BTAC)。5种季铵盐在质量浓度50～5000μg/L范围内具有良好的线性关系,相关系数r大于0.999,方法定量限为1.06～1.75mg/kg。空白基质加标回收试验添加水平分别为5、25和100 mg/kg时,化妆品中5种季铵盐的回收率在81.3%～115.6%之间,相对标准偏差≤5.0%。该方法灵敏度、精密度和定量限均符合实际样品检测要求,可用于化妆品中季铵盐的日常监测。
A rapid method for determining the quaternary ammonium salts in cosmetics by solid phase extraction-gas chromatography/mass spectrometry was developed. Five quaternary ammonium salts, including dodecyl trimethyl ammonium chloride(DTAC), alkyl trimethyl ammonium chloride(TTAC), hexadecyl trimethyl ammonium bromide(CTAB), octadecyl trimethyl ammonium chloride(STAC), and docosyl trimethyl ammonium chloride(BTAC) in cosmetics were simultaneously determined by electron bombardment(EI) and selective ion mode(SIM) with methanol as solvent, weak cation solid phase extraction and purification, and D9 hexadecyl trimethyl ammonium chloride as internal standard. It showed good linear relationship in the range of 50-5 000 g/L for ?ve quaternary ammonium salts, the correlation coef?cient was more than 0.999,and the quantitative limit was 1.06-1.75 mg/kg. The recoveries of ?ve quaternary ammonium salts in cosmetics ranged from81.3% to 111.6% and the relative standard deviation was less than 5.0% when the concentration of blank matrix was 5, 25 and 100 mg/kg, respectively. The sensitivity, precision and quantitative limit of the method were all in accordance with the requirements of actual samples, and it can be used for daily monitoring of quaternary ammonium salt in cosmetics.
A rapid method for determining the quaternary ammonium salts in cosmetics by solid phase extraction-gas chromatography/mass spectrometry was developed. Five quaternary ammonium salts, including dodecyl trimethyl ammonium chloride(DTAC), alkyl trimethyl ammonium chloride(TTAC), hexadecyl trimethyl ammonium bromide(CTAB), octadecyl trimethyl ammonium chloride(STAC), and docosyl trimethyl ammonium chloride(BTAC) in cosmetics were simultaneously determined by electron bombardment(EI) and selective ion mode(SIM) with methanol as solvent, weak cation solid phase extraction and purification, and D9 hexadecyl trimethyl ammonium chloride as internal standard. It showed good linear relationship in the range of 50-5 000 g/L for ?ve quaternary ammonium salts, the correlation coef?cient was more than 0.999,and the quantitative limit was 1.06-1.75 mg/kg. The recoveries of ?ve quaternary ammonium salts in cosmetics ranged from81.3% to 111.6% and the relative standard deviation was less than 5.0% when the concentration of blank matrix was 5, 25 and 100 mg/kg, respectively. The sensitivity, precision and quantitative limit of the method were all in accordance with the requirements of actual samples, and it can be used for daily monitoring of quaternary ammonium salt in cosmetics.
引文
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[11]NALECZ J G,GRABINSKA S E,NARKIEWICZ P.The toxicity of cationic surfacant in four bioassays[J].Ecotoxicology and Environmental Safety,2003,54(1):87-91.
[12]GARCIA M T,RIBOSA I,GUINDULAIN T.Fate and effect of monoalkyl quaternary ammonium surfactants in the aquatic environment[J].Environmental Pollution,2001,111(1):169-175.
[13]国家食品药品监督管理总局.化妆品安全技术规范[S].2015版.北京:中国标准出版社,2015.
[2]STEICHE D S.Cationic Surfactants[M]//HOLMBERG K.Handbook of Applied Surface and Colloid Chemistry.West Sussex:John Wiley&Sons,Ltd.,2001:309-314.
[3]PATRAUCHAN M A,ORIEL P J.Degradation of benzyldimethylalkylammonium chloride by Aeromonas hydrophila sp.K[J].Journal of Applied Microbiology,2003,94:266-272.
[4]TEZEL U.Fate and effect of quaternary ammonium compounds in biologica lsystems[D].Atlanta:Georgia Institute of Technology,2009.
[5]JING G,ZHOU Z,ZHOU J.Quantitative structure-activity relationship(QSAR)study of toxicity of quaternary ammonium compounds on Chlorella pyrenoidosa and Scenedesmus quadricauda[J].Chemosphere,2012,86:76-82.
[6]罗希权.2006年全国表面活性剂及其原料销量情况浅析[J].中国洗涤用品工业,2007(3):21-24.
[7]MARTINEZ C E,SITKA A,GONZALE B C,et al.Determination of selected quaternary ammonium compounds by liquid chromatography with mass spectrometry.Part I.Application to surface,waste and indirect discharge water samples in Austria[J].Environmental Pollution,2007,145:489-496.
[8]MARTINEZ C E,SITKA A,GONZALEZ B C,et al.Determination of selected quaternary ammonium compounds by liquid chromatography with mass spectrometry.Part II.Application to sediment and sludge samples in Austria[J].Environmental Pollution,2007,146:543-547.
[9]ISMAIL Z Z,TEZEL U,PAVLOSTATHIS S G.Sorption of quaternary ammonium compounds to municipal sludge[J].Water Research,2010,44:2303-2313.
[10]DE-VOORDE A V,LORGEOUX C,GROMAIRE M C,et al.Analysis of quaternary ammonium compounds in urban stormwater samples[J].Environmental Pollution,2012,164:150-157.
[11]NALECZ J G,GRABINSKA S E,NARKIEWICZ P.The toxicity of cationic surfacant in four bioassays[J].Ecotoxicology and Environmental Safety,2003,54(1):87-91.
[12]GARCIA M T,RIBOSA I,GUINDULAIN T.Fate and effect of monoalkyl quaternary ammonium surfactants in the aquatic environment[J].Environmental Pollution,2001,111(1):169-175.
[13]国家食品药品监督管理总局.化妆品安全技术规范[S].2015版.北京:中国标准出版社,2015.