UPLC-MS/MS测定化妆品中7种禁用物质残留
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摘要
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法同时测定化妆品中醋酸曲安奈德、氢化可的松、米诺地尔、螺内酯、坎利酮、雌酮、黄体酮等7种禁用物质残留。以Waters Acquity UPLC?BEH C18色谱柱(1.7μm×2.1 mm×50 mm)进行分离,以甲醇和0.2%甲酸水溶液为流动相梯度洗脱,流速为0.2 mL·min~(-1),进样量为1μL,采用多反应监测(MRM)扫描方式进行测定。在超高效液相色谱-串联质谱分析过程中以保留时间和离子对(母离子和两个子离子)信息比较定性,以母离子和响应值高的子离子进行定量。所建立的方法在相应的浓度范围内浓度和峰面积的线性关系良好,线性相关系数为0.999 5～0.9999,加标回收率在87.43%～99.24%(n=3)之间,相对标准偏差为1.25%～3.28%(n=6),检出限范围为0.041～3.26μg·kg~(-1),定量限范围为0.14～10.87μg·kg~(-1)。该方法准确、可靠,适用于化妆品中多种禁用物质的同时测定。
A method to determine 7 kinds of prohibited substances residues in cosmetics was established by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry(UPLC-MS/MS).Methods:The UPLC separation was carried out on a Waters Acquity UPLC~?BEH C18 column(1.7 μm × 2.1 mm ×50 mm)by gradient elution using methanol and 0.2%formic acid.The flow rate is 0.2 mL·min~(-1) and sample injection amount is 1 μL.The multiple reaction monitoring(MRM)scanning method was performed.Retention times and charge-mass ratio of compounds(parent ion and two daughter ions)were used for qualitative analysis,and the peak areas of parent ion and daughter ions on high intensity were used for quantitative analysis by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry.The established method has a good linear relationship betweenconcentration and peak area in the corresponding concentration range.The linear correlation coefficients were from 0.9995 to 0.9999.The recoveries were between 87.43%and 99.24%,and the relative standard deviations were from 1.25%to 3.28%.The detection limit were from 0.041 μg·kg~(-1) to 3.26 μg·kg~(-1).The limit of quantitation were from 0.14 μg·kg~(-1) to 10.87 μg·kg~(-1).In conclusion,the method had accurate and reliable detection results and was suitable for the simultaneous determination of various prohibited substances in cosmetics.
A method to determine 7 kinds of prohibited substances residues in cosmetics was established by Ultra Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry(UPLC-MS/MS).Methods:The UPLC separation was carried out on a Waters Acquity UPLC~?BEH C18 column(1.7 μm × 2.1 mm ×50 mm)by gradient elution using methanol and 0.2%formic acid.The flow rate is 0.2 mL·min~(-1) and sample injection amount is 1 μL.The multiple reaction monitoring(MRM)scanning method was performed.Retention times and charge-mass ratio of compounds(parent ion and two daughter ions)were used for qualitative analysis,and the peak areas of parent ion and daughter ions on high intensity were used for quantitative analysis by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry.The established method has a good linear relationship betweenconcentration and peak area in the corresponding concentration range.The linear correlation coefficients were from 0.9995 to 0.9999.The recoveries were between 87.43%and 99.24%,and the relative standard deviations were from 1.25%to 3.28%.The detection limit were from 0.041 μg·kg~(-1) to 3.26 μg·kg~(-1).The limit of quantitation were from 0.14 μg·kg~(-1) to 10.87 μg·kg~(-1).In conclusion,the method had accurate and reliable detection results and was suitable for the simultaneous determination of various prohibited substances in cosmetics.
引文
[1]张飞,华夏.化妆品中有毒有害物质污染现状及其检测方法研究进展[J].化工设计通讯,2018,44(5):215-253.
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[5]勾新磊,刘伟丽,张梅,等.超高效液相色谱-串联质谱法快速测定洗发育发类化妆品中6种违禁药物[J].质谱学报,2018,39(4):485-491.
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[10]冯学花,周娟,朱华燕.化妆品中禁限用成分检测方法研究概述[J].承德医学院学报,2017,34(1):85-87.
[11]孟宪双,马强,白桦,等.化妆品质量安全检测技术研究进展[J].分析测试学报,2016,35(2):143-155.
[12]刘齐,张华珺,郭洁,等.HPLC-MS/MS法同时测定育发液中的9种禁限用物质[J].药物分析杂志,2016,(9):1660-1666.
[13]戴明.UPLC-MS/MS法测定7类化妆品中4-氨基联苯[J].化学研究与应用,2013,(9):1314-1318.
[14]Feng X,Turley J,Xie Z,et al.An LC–MS/MS method for the determination of digitoxigenin in skin samples and its application to skin permeation and metabolic stability studies[J].J Pharmaceutical and Biomedical Analysis,2017,138:378-385.
[15]李疆,宋佳一,赵珊,等.化妆品中米诺地尔的毛细管区带电泳测定法[J].环境与健康杂志,2017,34(8):701-703.
[16]屈颖,唐素芳.高效液相色谱法测定螺内酯的有关物质[J].中国药品标准,2011,12(1):22-24.
[17]罗辉泰,黄晓兰,吴惠勤,等.分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素[J].色谱,2017,35(8):816-825.
[18]周智明,罗卓雅.液相色谱-串联质谱法测定化妆品中15种性激素[J].理化检验:化学分册,2018,54(2):161-166.
[19]岳磊,李晓静.超高效液相色谱-质谱联用法同时测定化妆品中5种禁用性激素[J].日用化学工业,2017,47(8):476-480.
[2]Guerra E,Alvarez-Rivera G,Llompart M,et al.Simultaneous determination of preservatives and synthetic dyes in cosmetics by single-step vortex extraction and clean-up followed by liquid chromatography coupled to tandem mass spectrometry[J].Talanta,2018(188):251-258.
[3]吴景,张凤兰,邢书霞,等.祛斑美白类化妆品质量现状分析及监管建议[J].中国卫生检验杂志,2016,(16):2429-2432.
[4]林志惠,赵彦,幸苑娜,等.超高效液相色谱-串联质谱法同时测定化妆品中21种性激素含量[J].试验室,2017,(4):441-447.
[5]勾新磊,刘伟丽,张梅,等.超高效液相色谱-串联质谱法快速测定洗发育发类化妆品中6种违禁药物[J].质谱学报,2018,39(4):485-491.
[6]吴景,邢书霞,王钢力.化妆品中非法添加禁用物质检测技术研究进展[J].日用化学品科学,2015,38(10):5-9.
[7]Lores M,Llompart M,Alvarez-Rivera G,et al.Positive lists of cosmetic ingredients:Analytical methodology for regulatory and safety controls-A review[J].Analytica Chimica Acta,2016,915:1-26.
[8]黄荣,叶峻,傅小红.化妆品及其原料中有毒残留物检测方法研究进展[J].日用化学工业,2014,44(1):39-44.
[9]陈金娣.化妆品质量安全检测技术及应用分析[J].化工管理,2018,(12):106-107.
[10]冯学花,周娟,朱华燕.化妆品中禁限用成分检测方法研究概述[J].承德医学院学报,2017,34(1):85-87.
[11]孟宪双,马强,白桦,等.化妆品质量安全检测技术研究进展[J].分析测试学报,2016,35(2):143-155.
[12]刘齐,张华珺,郭洁,等.HPLC-MS/MS法同时测定育发液中的9种禁限用物质[J].药物分析杂志,2016,(9):1660-1666.
[13]戴明.UPLC-MS/MS法测定7类化妆品中4-氨基联苯[J].化学研究与应用,2013,(9):1314-1318.
[14]Feng X,Turley J,Xie Z,et al.An LC–MS/MS method for the determination of digitoxigenin in skin samples and its application to skin permeation and metabolic stability studies[J].J Pharmaceutical and Biomedical Analysis,2017,138:378-385.
[15]李疆,宋佳一,赵珊,等.化妆品中米诺地尔的毛细管区带电泳测定法[J].环境与健康杂志,2017,34(8):701-703.
[16]屈颖,唐素芳.高效液相色谱法测定螺内酯的有关物质[J].中国药品标准,2011,12(1):22-24.
[17]罗辉泰,黄晓兰,吴惠勤,等.分散固相萃取-液相色谱-串联质谱法同时快速测定化妆品中81种糖皮质激素[J].色谱,2017,35(8):816-825.
[18]周智明,罗卓雅.液相色谱-串联质谱法测定化妆品中15种性激素[J].理化检验:化学分册,2018,54(2):161-166.
[19]岳磊,李晓静.超高效液相色谱-质谱联用法同时测定化妆品中5种禁用性激素[J].日用化学工业,2017,47(8):476-480.