超高效液相色谱-串联质谱法测定婴幼儿化妆品中米诺地尔等7种成分
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摘要
目的对市售婴幼儿化妆品中米诺地尔、氢化可的松、螺内酯、雌酮、坎利酮、醋酸曲安奈德、黄体酮7种禁用成分进行市场调研。方法以Atlantis dC_(18) (100 mm×2.1 mm, 2μm)为分析柱, 0.1%甲酸溶液-甲醇为流动相进行梯度洗脱后,采用超高效液相色谱-串联质谱电喷雾电离(ESI+)检测7种禁用成分。结果 7种标准溶液在10～600ng浓度范围内呈良好线性关系(r≥0.9990),加标回收率为92.6%～95.2%,相对标准偏差(relative standard deviations, RSDs)为2.1%～4.1%,对20批市售婴幼儿化妆品中米诺地尔等7种成分进行检测,结果均未检出。结论我省婴幼儿化妆品市场中米诺地尔等7种成分的市场现状相对良好。
Objective To investigate 7 kinds of banned ingredients(minoxidil, hydrocortisone, spironolactone,estrone, canalidone, triamcinolone acetate, and progesterone) in infant cosmetics on the market. Methods Seven kinds of banned ingredients were detected by ultra-high performance liquid chromatography-tandem mass spectrometry electrospray ionization(ESI+), using a column of Atlantis dC_(18)(100 mm×2.1 mm, 2 μm), with the mobile phase of 0.1% formic acid solution for gradient elution. Results The 7 standard solutions showed good linear relationships(r≥0.9990) in the concentration range of 10-600 ng. The recoveries of the spiked concentrations were 92.6%-95.2% and relative standard deviations(RSDs) were 2.1%-4.1%. The 7 components in 20 batches of cosmetics for infants and young children were not detected. Conclusion The market situation of minoxidil and other 6 ingredients in infant cosmetics market in our province is relatively good.
Objective To investigate 7 kinds of banned ingredients(minoxidil, hydrocortisone, spironolactone,estrone, canalidone, triamcinolone acetate, and progesterone) in infant cosmetics on the market. Methods Seven kinds of banned ingredients were detected by ultra-high performance liquid chromatography-tandem mass spectrometry electrospray ionization(ESI+), using a column of Atlantis dC_(18)(100 mm×2.1 mm, 2 μm), with the mobile phase of 0.1% formic acid solution for gradient elution. Results The 7 standard solutions showed good linear relationships(r≥0.9990) in the concentration range of 10-600 ng. The recoveries of the spiked concentrations were 92.6%-95.2% and relative standard deviations(RSDs) were 2.1%-4.1%. The 7 components in 20 batches of cosmetics for infants and young children were not detected. Conclusion The market situation of minoxidil and other 6 ingredients in infant cosmetics market in our province is relatively good.
引文
[1]裘炳毅,高志红.现代化妆品科学与技术[M].北京:中国轻工业出版社,2016.Qiu BY,Gao ZH.Modern cosmetics science and technology[M].Beijing:China Light Industry Press,2016.
[2]国家食品药品监督管理总局.广西壮族自治区食品药品监督管理局关于2016年广西化妆品质量监督抽检结果公告[EB/OL].[2016-08].http://www.nmpa.gov.cn/WS04/CL2124/282122.html.State Food and Drug Administration.Guangxi Zhuang Autonomous Region Food and Drug Administration Announcement on the results of2016 Guangxi cosmetics quality supervision and inspection[EB/OL].[2016-08].http://www.nmpa.gov.cn/WS04/CL2124/282122.html.
[3]国家食品药品监督管理总局.转河南省食品药品监督管理局化妆品监督抽检结果公告[EB/OL].[2017-01].http://www.nmpa.gov.cn/WS04/CL2124/282150.html.State Food and Drug Administration.Announcement of results of cosmetics supervision and sampling inspection of Henan Food and Drug Administration[EB/OL].[2017-01].http://www.nmpa.gov.cn/WS04/CL2124/282150.html.
[4]国家食品药品监督管理总局.化妆品安全技术规范(2015版)[S].State Food and Drug Administration.Technical specification for cosmetic safety(2015 edition)[S].
[5]郑磊,胡小键,林少彬.育发产品中斑蝥素和氮芥及米诺地尔的液相色谱-串联质谱测定法[J].环境与健康杂志,2016,33(1):66-68.Zheng L,Hu XJ,Lin SB.Determination of cantharidin,nitrogen mustard and minoxidil in hair products by liquid chromatography-tandem mass spectrometry[J].J Environ Health,2016,33(1):66-68.
[6]李仙玉.短期氢化可的松治疗小儿肺部支原体感染诱发大叶性肺炎的疗效观察[J].中国民康医学,2016,28(16):16-17.Li XY.Observation on the efficacy of short-term hydrocortisone in the treatment of lobar pneumonia induced by mycoplasma pulmonale infection in children[J].Minkang Med China,2016,28(16):16-17.
[7]潘小红,殷帅,刘玉玲,等.全自动固相萃取-高效液相色谱-串联质谱法测定婴幼儿产品中42种糖皮质激素[J].色谱,2018,36(4):356-361.Pan XH,Yin S,Liu YL,et al.Fully automatic solid phase extraction-high performance liquid chromatography-tandem mass spectrometry for the determination of 42 glucocorticoids in infant products[J].Chin JChromatogr,2018,36(4):356-361.
[8]左晓玥.婴儿湿疹的护理[J].当代临床医刊,2015,6(28):1820-1821.Zuo XY.Nursing of infantile eczema[J].Contemp Clin J,2015,6(28):1820-1821.
[9]梁雪梅,刘亚辉,钟维林.不同剂量螺内酯对难治性心力衰竭患者心功能的治疗效果差异[J].临床研究,2015,13(31):143.Liang XM,Liu YH,Zhong WL.The difference of therapeutic effect of different doses of spironolactone on cardiac function in patients with refractory heart failure[J].Clin Study,2015,13(31):143.
[10]陈敏,蒋雯.螺内酯对慢性心力衰竭患者心脏自主神经功能的影响[J].中国医院药学杂志,2016,36(22):2004-2007.Chen M,Jiang W.Effects of spironolactone on cardiac autonomic nervous function in patients with chronic heart failure[J].Chin J Hosp Pharm,2016,36(22):2004-2007.
[11]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].日用化学化工,2017,8(47):476-480.Yue L,Li XJ.Simultaneous determination of five prohibited hormones in cosmetics by ultra-high performance liquid chromatography-mass spectrometry[J].Daily Chem Ind,2017,8(47):476-480.
[12]张道惠.黄体酮治疗早期流产的疗效及对围生儿结局的影响[J].深圳中西医结合杂志,2016,2(4):23-25.Zhang DH.Effect of progesterone on early abortion and perinatal outcome[J].Shenzhen J Integr Tradit Chin West Med,2016,2(4):23-25.
[13]袁洁,周晨忱,姚军.LC-MS/MS法测定新疆市场鸡肝中棉酚旋光异构体[J].分析试验室,2016,35(11):1250-1253.Yuan J,Zhou CC,Yao J.LC-MS/MS determination of gossypol optical isomers in chicken liver of Xinjiang market[J].Anal Lab,2016,35(11):1250-1253.
[14]王霄旸,张可煜,张丽芳,等.利用UPLC-TOF及MS/MS鉴定头孢喹肟中的同分异构体[J].中国兽医科学,2016,46(5):623-629.Wang XY,Zhang KY,Zhang LF,et al.Identification of isomer in cefquinoxime by UPLC-TOF and MS/MS[J].Chin Vet Sci,2016,46(5):623-629.
[15]Laine JE,Auriola S,Pasanen M,et al.D-Isomer of gly-tyrpro-cys-pro-his-pro peptide:A novel and sensitive in vitro trapping agent to detect reactive metabolites by electrospray mass spectrometry[J].Toxicol in Vitro,2011,25(1):411-425.
[16]Kocadagli T,Yilmaz C,Gokmen V.Determination of melatonin and its isomer in foods by liquid chromatography tandem mass spectrometry[J].Food Chem,2014,(153):151-156.
[17]Qian JQ,Correra TC,Li J,et al.Differentiation of cefaclor and its delta-3isomer by electrospray mass spectrometry,infrared multiple photon dissociation spectroscopy and theoretical calculations[J].J Mass Spectrom,2015,50(1):265-269.
[18]罗辉泰,黄晓兰,吴惠勤,等.固相萃取/液相色谱-串联质谱法同时测定面膜类化妆品中非法添加的53种糖皮质激素[J].分析测试学报,2016,35(2):119-126.Luo HT,Huang XL,Wu HQ,et al.Simultaneous determination of 53glucocorticoids illegally added to mask cosmetics by solid phase extraction/liquid chromatography tandem mass spectrometry[J].J Anal Test,2016,35(2):119-126.
[2]国家食品药品监督管理总局.广西壮族自治区食品药品监督管理局关于2016年广西化妆品质量监督抽检结果公告[EB/OL].[2016-08].http://www.nmpa.gov.cn/WS04/CL2124/282122.html.State Food and Drug Administration.Guangxi Zhuang Autonomous Region Food and Drug Administration Announcement on the results of2016 Guangxi cosmetics quality supervision and inspection[EB/OL].[2016-08].http://www.nmpa.gov.cn/WS04/CL2124/282122.html.
[3]国家食品药品监督管理总局.转河南省食品药品监督管理局化妆品监督抽检结果公告[EB/OL].[2017-01].http://www.nmpa.gov.cn/WS04/CL2124/282150.html.State Food and Drug Administration.Announcement of results of cosmetics supervision and sampling inspection of Henan Food and Drug Administration[EB/OL].[2017-01].http://www.nmpa.gov.cn/WS04/CL2124/282150.html.
[4]国家食品药品监督管理总局.化妆品安全技术规范(2015版)[S].State Food and Drug Administration.Technical specification for cosmetic safety(2015 edition)[S].
[5]郑磊,胡小键,林少彬.育发产品中斑蝥素和氮芥及米诺地尔的液相色谱-串联质谱测定法[J].环境与健康杂志,2016,33(1):66-68.Zheng L,Hu XJ,Lin SB.Determination of cantharidin,nitrogen mustard and minoxidil in hair products by liquid chromatography-tandem mass spectrometry[J].J Environ Health,2016,33(1):66-68.
[6]李仙玉.短期氢化可的松治疗小儿肺部支原体感染诱发大叶性肺炎的疗效观察[J].中国民康医学,2016,28(16):16-17.Li XY.Observation on the efficacy of short-term hydrocortisone in the treatment of lobar pneumonia induced by mycoplasma pulmonale infection in children[J].Minkang Med China,2016,28(16):16-17.
[7]潘小红,殷帅,刘玉玲,等.全自动固相萃取-高效液相色谱-串联质谱法测定婴幼儿产品中42种糖皮质激素[J].色谱,2018,36(4):356-361.Pan XH,Yin S,Liu YL,et al.Fully automatic solid phase extraction-high performance liquid chromatography-tandem mass spectrometry for the determination of 42 glucocorticoids in infant products[J].Chin JChromatogr,2018,36(4):356-361.
[8]左晓玥.婴儿湿疹的护理[J].当代临床医刊,2015,6(28):1820-1821.Zuo XY.Nursing of infantile eczema[J].Contemp Clin J,2015,6(28):1820-1821.
[9]梁雪梅,刘亚辉,钟维林.不同剂量螺内酯对难治性心力衰竭患者心功能的治疗效果差异[J].临床研究,2015,13(31):143.Liang XM,Liu YH,Zhong WL.The difference of therapeutic effect of different doses of spironolactone on cardiac function in patients with refractory heart failure[J].Clin Study,2015,13(31):143.
[10]陈敏,蒋雯.螺内酯对慢性心力衰竭患者心脏自主神经功能的影响[J].中国医院药学杂志,2016,36(22):2004-2007.Chen M,Jiang W.Effects of spironolactone on cardiac autonomic nervous function in patients with chronic heart failure[J].Chin J Hosp Pharm,2016,36(22):2004-2007.
[11]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].日用化学化工,2017,8(47):476-480.Yue L,Li XJ.Simultaneous determination of five prohibited hormones in cosmetics by ultra-high performance liquid chromatography-mass spectrometry[J].Daily Chem Ind,2017,8(47):476-480.
[12]张道惠.黄体酮治疗早期流产的疗效及对围生儿结局的影响[J].深圳中西医结合杂志,2016,2(4):23-25.Zhang DH.Effect of progesterone on early abortion and perinatal outcome[J].Shenzhen J Integr Tradit Chin West Med,2016,2(4):23-25.
[13]袁洁,周晨忱,姚军.LC-MS/MS法测定新疆市场鸡肝中棉酚旋光异构体[J].分析试验室,2016,35(11):1250-1253.Yuan J,Zhou CC,Yao J.LC-MS/MS determination of gossypol optical isomers in chicken liver of Xinjiang market[J].Anal Lab,2016,35(11):1250-1253.
[14]王霄旸,张可煜,张丽芳,等.利用UPLC-TOF及MS/MS鉴定头孢喹肟中的同分异构体[J].中国兽医科学,2016,46(5):623-629.Wang XY,Zhang KY,Zhang LF,et al.Identification of isomer in cefquinoxime by UPLC-TOF and MS/MS[J].Chin Vet Sci,2016,46(5):623-629.
[15]Laine JE,Auriola S,Pasanen M,et al.D-Isomer of gly-tyrpro-cys-pro-his-pro peptide:A novel and sensitive in vitro trapping agent to detect reactive metabolites by electrospray mass spectrometry[J].Toxicol in Vitro,2011,25(1):411-425.
[16]Kocadagli T,Yilmaz C,Gokmen V.Determination of melatonin and its isomer in foods by liquid chromatography tandem mass spectrometry[J].Food Chem,2014,(153):151-156.
[17]Qian JQ,Correra TC,Li J,et al.Differentiation of cefaclor and its delta-3isomer by electrospray mass spectrometry,infrared multiple photon dissociation spectroscopy and theoretical calculations[J].J Mass Spectrom,2015,50(1):265-269.
[18]罗辉泰,黄晓兰,吴惠勤,等.固相萃取/液相色谱-串联质谱法同时测定面膜类化妆品中非法添加的53种糖皮质激素[J].分析测试学报,2016,35(2):119-126.Luo HT,Huang XL,Wu HQ,et al.Simultaneous determination of 53glucocorticoids illegally added to mask cosmetics by solid phase extraction/liquid chromatography tandem mass spectrometry[J].J Anal Test,2016,35(2):119-126.