液相色谱-串联质谱法测定儿童化妆品中3种异噻唑啉酮类防腐剂
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摘要
建立了儿童化妆品中防腐剂异噻唑啉酮类化合物的液相色谱-串联质谱(LC-MS/MS)测定方法。采用Waters Symmetry?C18色谱柱(150×2.1mm,3.5μm);流动相为甲醇-0.1%甲酸溶液(45∶55,V/V),等度洗脱,流速200μL/min,在选择反应监测(SRM)模式下定性和定量分析。定量结果表明,3种异噻唑啉酮防腐剂的浓度在5～2 000μg/L范围内与其峰面积呈现良好的线性关系,其线性相关系数均≥0.9999,方法的检出限和定量限满足国内外现行的化妆品安全法规对这3种防腐剂的限量要求。方法平均回收率为94.0%～105.6%,相对标准偏差均小于5%(n=6)。
A sensitive and rapid method was developed for the determination of three isothiazolinone preservatives in children cosmetics by high-performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analysis were performed on Waters Symmetry?C18column(150×2.1mm,3.5μm)under the isocratic elution of methanol and 0.1%formic acid solution(45∶55,V/V),and in selected-reaction monitoring(SRM)mode in this method.The flow rate was set at 200μL/min.The results displayed that three kinds of compounds showed good linearity within the concentration range of 5-2 000μg/L.The corresponding linear correlation coefficients were all equal to or greater than 0.9999.And the limits of detection and limits of quantification could meet the detection requirements of the current lays and regulation of cosmetics around the world.The recoveries were between 94.0% and 105.6% with relative standard deviations<5%(n=6).
A sensitive and rapid method was developed for the determination of three isothiazolinone preservatives in children cosmetics by high-performance liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analysis were performed on Waters Symmetry?C18column(150×2.1mm,3.5μm)under the isocratic elution of methanol and 0.1%formic acid solution(45∶55,V/V),and in selected-reaction monitoring(SRM)mode in this method.The flow rate was set at 200μL/min.The results displayed that three kinds of compounds showed good linearity within the concentration range of 5-2 000μg/L.The corresponding linear correlation coefficients were all equal to or greater than 0.9999.And the limits of detection and limits of quantification could meet the detection requirements of the current lays and regulation of cosmetics around the world.The recoveries were between 94.0% and 105.6% with relative standard deviations<5%(n=6).
引文
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[3] CHEN Y C,XIE X B,SHI Q S,et al.Fine and Specialty Chemicals(陈艺彩,谢小保,施庆珊,等.精细与专用化学品),2010,18(1):43.
[4] García-Gavín J,Vansina S,Kerre S,Naert A,Goossens A.Contact Dermatitis,2010,63(2):96.
[5] SI X S,YANG J W,HANG L.Applied Chemical Industry(司新生,杨俊伟,杭磊.应用化工),2011,40(10):1789.
[6] LIN F,MAO S L,CHEN B,et al.China Leather(林芳,毛树禄,陈斌,等.中国皮革),2011,40(7):5.
[7] Naresh M P,Eyal S,Susan R,Daniel J G,Rachel G,Helaine E R.American Journal of Epidemiology,2004,160(6):521.
[8] European Parliament,Council,Regulation,EC:1223/2009[EB/OL].http://eur-lex.europa.eu/legal-content/EN/TXT/HTML/?uri=CELEX:32009R1223&qid=1537838397302&from=EN.
[9] EN 71-9-2005:Safety of Toys-Part 9:Organic Chemical Compounds-Requirement.
[10]Regulation(EU)No.528/2012of the European Parliament and of the Council of 22 May 2012Concerning the Making Available on the Market and Use of Biocidal Products.Official Journal of the European Union,2012,L167:1.
[11]中华人民共和国食品药品监督管理总局:Safety and Technical Standards for Cosmetics(2015Version)(化妆品安全技术规范(2015版)).
[12]Commission Regulation(EU)2016/1198of 22July 2016amending Annex V to Regulation(EC)No 1223/2009of the European Parliament and of the Council on Cosmetic Products[EB/OL].[2016-07-22].http://eur-lex.europa.eu/legal content/EN/TXT/?uri=uriserv%3AOJ.L_.2016.198.01.0010.01.ENG.
[13]SUN X Q,WANG T,WANG S M.Detergent&Cosmetics(孙晓青,王彤,王粟明.日用化学品科学),2017,40(2):26.
[14]ZHANG J M,PAN Y N,BAI H.Industrial Water Treatment(张建玫,潘亚男,白桦.工业水处理),2011,31(5):70.
[15]ZHENG J,CHEN Y Q,GONG C,et al.Journal of Zhengzhou University(Natural Science Edition)(郑静,陈燕青,龚晨,等.郑州大学学报(理学版)),2011,43(1):122-124.
[16]SUN Z S,DU H Q,LIU B,et al.Journal of Instrumental Analysis(孙忠松,杜恒清,刘宝,等.分析测试学报),2012,31(supp1):67.
[17]Nakashima H,Matsunaga I,Miyano N,Kitagawa M.Journal of Health Science,2000,46(6):447.
[18]JI H W,DONG R,LIU J,et al.Physical Testing and Chemical Analysis Part B:Chemical Analysis(姬厚伟,董睿,刘剑,等.理化检验-化学分册),2017,53(4):432.
[19]Lin Q B,Wang T J,Song H,Li B.Food Additives&Contaminants Part A-Chemistry Analysis Control Exposure&Risk Assessment,2010,27(12):1775.
[20]SN/T 2404-2009:Determination of 2-Methyl-4-isothiazolin-3-one and Its Derivatives in Toys(玩具中防腐剂2-甲基-4-异噻唑啉-3-酮及其衍生物的测定).