超高效液相色谱-差分离子淌度质谱法测定化妆品中10种卡因类禁用组分
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摘要
建立了化妆品中10种卡因类禁用组分的超高效液相色谱-差分离子淌度质谱测定方法。以正十二醇为萃取剂、四氢呋喃为分散剂在水中自组装形成超分子溶剂,并结合涡旋辅助对化妆品试样进行分散液液微萃取。考察了超分子溶剂的组成、用量及涡旋时间等参数对萃取效率的影响,以及差分离子淌度质谱对同分异构体的分离效果。结果表明,试样在4 mL正十二醇-四氢呋喃超分子溶剂中涡旋振荡3 min即可完成高效萃取,且可有效去除基质干扰,降低基质效应。差分离子淌度质谱在优化的载气、分离电压、补偿电压等条件下可将色谱难以分离的同分异构体(苯佐卡因和三卡因)实现淌度分离,解决了两种同分异构体由于色谱无法分离而不能准确定性和定量分析的问题。10种卡因类组分在各自浓度范围内线性关系良好,相关系数均大于0.99,方法检出限为0.2～8.0μg/kg,方法定量限为0.4～20.0μg/kg。在低、中、高3个添加水平下的平均回收率为70.7%～94.7%,相对标准偏差为1.2%～12.7%(n=6)。本方法步骤简便、快速高效,适用于化妆品中10种卡因类禁用组分的同时分析测定。
An analytical method for determination of 10 kinds of caine-type prohibited ingredients in cosmetics was developed using supramolecular solvent-based dispersive liquid-liquid microextraction followed by ultra-performance liquid chromatography coupled with differential mobility spectrometry-mass spectrometry. The supramolecular solvent was prepared with dodecanol as extraction solvent and tetrahydrofuran as dispersing agent for dispersive liquid-liquid microextraction of cosmetic samples under vortexing. The effects of the composition and amount of supramolecular solvent and vortex time on the extraction efficiency and the separation of isomers by differential mobility spectrometry were systemitically investigated. Results showed that the sample could be effectively extracted by 4 mL of supramolecular solvent consisting of dodecanol and tetrahydrofuran after vortexing for 3 min. Under the optimized conditions including carrier gas, separation voltage and compensation voltage, the isomers of benzocaine and tricaine could be well separated by differential mobility spectrometry for qualitative confirmation and quantitative determination, which could hardly be chromatographically separated. The 10 kinds of caine-type compounds exhibited good linearity in their respective concentration ranges, with correlation coefficients of better than 0.99. The limits of detection and quantitation were 0.2-8.0 μg/kg and 0.4-20.0 μg/kg, respectively. The average recoveries at low, medium and high spiked levels ranged from 70.7% to 94.7% with relative standard deviations of 1.2% to 12.7%(n=6). The method is simple, rapid, efficient, and is suitable for the simultaneous determination of the 10 kinds of caine-type prohibited ingredients in cosmetics.
An analytical method for determination of 10 kinds of caine-type prohibited ingredients in cosmetics was developed using supramolecular solvent-based dispersive liquid-liquid microextraction followed by ultra-performance liquid chromatography coupled with differential mobility spectrometry-mass spectrometry. The supramolecular solvent was prepared with dodecanol as extraction solvent and tetrahydrofuran as dispersing agent for dispersive liquid-liquid microextraction of cosmetic samples under vortexing. The effects of the composition and amount of supramolecular solvent and vortex time on the extraction efficiency and the separation of isomers by differential mobility spectrometry were systemitically investigated. Results showed that the sample could be effectively extracted by 4 mL of supramolecular solvent consisting of dodecanol and tetrahydrofuran after vortexing for 3 min. Under the optimized conditions including carrier gas, separation voltage and compensation voltage, the isomers of benzocaine and tricaine could be well separated by differential mobility spectrometry for qualitative confirmation and quantitative determination, which could hardly be chromatographically separated. The 10 kinds of caine-type compounds exhibited good linearity in their respective concentration ranges, with correlation coefficients of better than 0.99. The limits of detection and quantitation were 0.2-8.0 μg/kg and 0.4-20.0 μg/kg, respectively. The average recoveries at low, medium and high spiked levels ranged from 70.7% to 94.7% with relative standard deviations of 1.2% to 12.7%(n=6). The method is simple, rapid, efficient, and is suitable for the simultaneous determination of the 10 kinds of caine-type prohibited ingredients in cosmetics.
引文
1 ZHANG Yan-Shu,LIN Zhen-Hua,HU Yu-Ling,LI Gong-Ke.Journal of Instrumental Analysis,2016,35(2):127-136张艳树,林振华,胡玉玲,李攻科.分析测试学报,2016,35(2):127-136
2 XU Yin-Yu.Chemical Enterprise Management,2018,(16):38-39许银玉.化工管理,2018,(16):38-39
3 ZHANG Qing-Sheng,WANG Gang-Li.Cosmetic Safety Technical Specification.Beijing:People's Medical Publishing House,2017:238-244张庆生,王钢力.化妆品安全技术规范.北京:人民卫生出版社,2017:238-244
4 Regulation (EC) No.1223/2009 of the European Parliament and of the Council of 30 November 2009 on Cosmetic Products.Official Journal of the European Union,2009,https://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2009:342:0059:0209:en:PDF
5 Health Products (Cosmetic Products - ASEAN Cosmetic Directive) Regulations 2007,https://sso.agc.gov.sg/SL/HPA2007-S683-2007
6 LI Wei,RUI Chang,TU Hai-Yun,ZHAO Kai,WANG Xiao,ZHOU Min,WANG Na.Chinese Journal of Analysis Laboratory,2011,30(12):85-89李玮,芮昶,屠海云,赵凯,王啸,周敏,王娜.分析试验室,2011,30(12):85-89
7 XIAO Xiao-Hua,YIN Yi,HU Yu-Ling,LI Gong-Ke.Chinese Journal of Chromatography,2007,25(2):234-237肖小华,尹怡,胡玉玲,李攻科.色谱,2007,25(2):234-237
8 WANG Yan-Qin,CHE Wen-Jun,WANG Li,XU Chun-Xiang,LU Jian.Chinese J.Anal.Chem.,2013,41(3):394-399王燕芹,车文军,王莉,徐春祥,卢剑.分析化学,2013,41(3):394-399
9 SHEN Hao-Yu,YING Li-Yan,CAO Yun-Feng,PAN Gang,ZHOU Lu.Chinese Journal of Chromatography,2007,25(2):272-275沈昊宇,应丽艳,曹云峰,潘刚,周鹿.色谱,2007,25(2):272-275
10 Aydin F,Yilmaz E,Soylak M.RSC Adv.,2015,5(50):40422-40428
11 Ballesteros-Gómez A,Rubio S,Pérez-Bendito D.J.Chromatogr.A,2009,1216(3) :530-539
12 Caballo C,Sicilia M D,Rubio S.Application of Green Solvents in Seperation Process.Elsevier Inc.,2017:111-137
13 Ballesteros-Gómez A,Sicilia M D,Rubio S.Anal.Chim.Acta,2010,677(2):108-130
14 López-Jiméz F J,Lunar M L,Sicila M D,Rubio S.Supramolecular Solvents in the Analytica.Encyclopedia of Analytical Chemistry.Hoboken:John Wiley & Sons,Ltd,2014:1-16
15 Taiwan Society for Mass Spectrometry.Principles and Applications of Mass Spectrometry.Beijing:Science Press,2019,1:161-162 台湾质谱学会.质谱分析技术与应用.北京:科学出版社,2019,1:161-162
16 WANG Yu-Na,MENG Xian-Shuang,LIU Li-Juan,BAI Hua,MA Qiang.Journal of Instrumental Analysis,2018,37(10):1130-1138王玉娜,孟宪双,刘丽娟,白桦,马强.分析测试学报,2018,37(10):1130-1138
17 LI Chun-Bo.Modern Scientific Instruments.2011,(5):163-165李春波.现代科学仪器,2011,(5):163-165
18 Chen P S ,Chen S H ,Chen J H,Haung W Y,Liu H T,Kong P H,Yang O H.Anal.Chim.Acta,2016,946:1-8
19 Fu Y,Xia Y Q,Flarakos J,Tse F L,Miller J D,Jones E B,Li W.Anal.Chem.,2016,88(7):3655-3661
20 Ren T,Li R,Meng X,Fawcett J P,Sun D,Gu J.J.Pharm.Biomed.Anal.,2018,151:260-265
21 Nie J,Miao S,Lehotay S J,Li W T,Zhou H,Mao X H,Lu J W,Lan L,Ji S.Food Addit.Contam.A,2015,32(8):1287-1300
22 García-Fonseca S,Rubio S.Talanta,2016,148:370-379
23 TIAN Yu-Ping,GU Ling-Ling.Shanghai Measurement and Testing,2015,42(5):10-11田玉平,顾玲玲.上海计量测试,2015,42(5):10-11
24 WANG Huan,HU Lei,ZHOU Ming-Hao.Detergent & Cosmetics,2017,40(9):30-34王欢,胡磊,周明昊.日用化学品科学,2017,40(9):30-34
2 XU Yin-Yu.Chemical Enterprise Management,2018,(16):38-39许银玉.化工管理,2018,(16):38-39
3 ZHANG Qing-Sheng,WANG Gang-Li.Cosmetic Safety Technical Specification.Beijing:People's Medical Publishing House,2017:238-244张庆生,王钢力.化妆品安全技术规范.北京:人民卫生出版社,2017:238-244
4 Regulation (EC) No.1223/2009 of the European Parliament and of the Council of 30 November 2009 on Cosmetic Products.Official Journal of the European Union,2009,https://eur-lex.europa.eu/LexUriServ/LexUriServ.do?uri=OJ:L:2009:342:0059:0209:en:PDF
5 Health Products (Cosmetic Products - ASEAN Cosmetic Directive) Regulations 2007,https://sso.agc.gov.sg/SL/HPA2007-S683-2007
6 LI Wei,RUI Chang,TU Hai-Yun,ZHAO Kai,WANG Xiao,ZHOU Min,WANG Na.Chinese Journal of Analysis Laboratory,2011,30(12):85-89李玮,芮昶,屠海云,赵凯,王啸,周敏,王娜.分析试验室,2011,30(12):85-89
7 XIAO Xiao-Hua,YIN Yi,HU Yu-Ling,LI Gong-Ke.Chinese Journal of Chromatography,2007,25(2):234-237肖小华,尹怡,胡玉玲,李攻科.色谱,2007,25(2):234-237
8 WANG Yan-Qin,CHE Wen-Jun,WANG Li,XU Chun-Xiang,LU Jian.Chinese J.Anal.Chem.,2013,41(3):394-399王燕芹,车文军,王莉,徐春祥,卢剑.分析化学,2013,41(3):394-399
9 SHEN Hao-Yu,YING Li-Yan,CAO Yun-Feng,PAN Gang,ZHOU Lu.Chinese Journal of Chromatography,2007,25(2):272-275沈昊宇,应丽艳,曹云峰,潘刚,周鹿.色谱,2007,25(2):272-275
10 Aydin F,Yilmaz E,Soylak M.RSC Adv.,2015,5(50):40422-40428
11 Ballesteros-Gómez A,Rubio S,Pérez-Bendito D.J.Chromatogr.A,2009,1216(3) :530-539
12 Caballo C,Sicilia M D,Rubio S.Application of Green Solvents in Seperation Process.Elsevier Inc.,2017:111-137
13 Ballesteros-Gómez A,Sicilia M D,Rubio S.Anal.Chim.Acta,2010,677(2):108-130
14 López-Jiméz F J,Lunar M L,Sicila M D,Rubio S.Supramolecular Solvents in the Analytica.Encyclopedia of Analytical Chemistry.Hoboken:John Wiley & Sons,Ltd,2014:1-16
15 Taiwan Society for Mass Spectrometry.Principles and Applications of Mass Spectrometry.Beijing:Science Press,2019,1:161-162 台湾质谱学会.质谱分析技术与应用.北京:科学出版社,2019,1:161-162
16 WANG Yu-Na,MENG Xian-Shuang,LIU Li-Juan,BAI Hua,MA Qiang.Journal of Instrumental Analysis,2018,37(10):1130-1138王玉娜,孟宪双,刘丽娟,白桦,马强.分析测试学报,2018,37(10):1130-1138
17 LI Chun-Bo.Modern Scientific Instruments.2011,(5):163-165李春波.现代科学仪器,2011,(5):163-165
18 Chen P S ,Chen S H ,Chen J H,Haung W Y,Liu H T,Kong P H,Yang O H.Anal.Chim.Acta,2016,946:1-8
19 Fu Y,Xia Y Q,Flarakos J,Tse F L,Miller J D,Jones E B,Li W.Anal.Chem.,2016,88(7):3655-3661
20 Ren T,Li R,Meng X,Fawcett J P,Sun D,Gu J.J.Pharm.Biomed.Anal.,2018,151:260-265
21 Nie J,Miao S,Lehotay S J,Li W T,Zhou H,Mao X H,Lu J W,Lan L,Ji S.Food Addit.Contam.A,2015,32(8):1287-1300
22 García-Fonseca S,Rubio S.Talanta,2016,148:370-379
23 TIAN Yu-Ping,GU Ling-Ling.Shanghai Measurement and Testing,2015,42(5):10-11田玉平,顾玲玲.上海计量测试,2015,42(5):10-11
24 WANG Huan,HU Lei,ZHOU Ming-Hao.Detergent & Cosmetics,2017,40(9):30-34王欢,胡磊,周明昊.日用化学品科学,2017,40(9):30-34