中国食品药品检定研究院,国家药品监督管理局化妆品研究与评价重点实验室,北京 100050
王海燕,博士,研究员,研究方向:化妆品安全检测新方法和新技术,E-mail: Summerwhy163@163.com
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董亚蕾,乔亚森,黄传峰等.超高效液相色谱-串联质谱法测定化妆品中的6种镇痛类化学成分[J].分析测试学报,2022,41(02):220-226.
DONG Ya-lei,QIAO Ya-sen,HUANG Chuan-feng,et al.Determination of 6 Analgesic Drugs in Cosmetics by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):220-226.
董亚蕾,乔亚森,黄传峰等.超高效液相色谱-串联质谱法测定化妆品中的6种镇痛类化学成分[J].分析测试学报,2022,41(02):220-226. DOI: 10.19969/j.fxcsxb.21042902.
DONG Ya-lei,QIAO Ya-sen,HUANG Chuan-feng,et al.Determination of 6 Analgesic Drugs in Cosmetics by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2022,41(02):220-226. DOI: 10.19969/j.fxcsxb.21042902.
建立了同时测定化妆品中氨基比林、非那西丁、双氯芬酸钠、吲哚美辛、保泰松、氯苯那敏等6种镇痛类化学成分含量的超高效液相色谱-串联质谱(UHPLC-MS/MS)法。以膏霜、面膜、啫喱和喷雾类样品为代表性基质,化妆品样品采用乙腈进行超声辅助液液萃取,采用ACQUITY UPLC BEH C,18,柱(2.1 mm × 100 mm,1.7 μm)分离,以含5 mmol/L乙酸铵的乙腈和水为流动相进行梯度洗脱,在多反应监测(MRM)模式下,通过串联质谱检测器进行检测。结果表明,6种化合物在5 ~ 200 μg/L范围内线性关系良好,相关系数(,r,)均大于0.99,检出限和定量下限分别为0.15 μg/g和0.50 μg/g。低、中、高3个浓度水平的加标回收率为75.0% ~ 120%,日内相对标准偏差(RSD)均不大于7.9%,日间RSD均不大于9.7%。该方法操作简便、灵敏度高、准确性好,适用于化妆品中镇痛类化学成分含量的检测,可为化妆品安全监管提供技术支撑。
A method was developed for the simultaneous determination of six illegally added analgesic drugs,i.e aminopyrine,phenacetin,diclofenac sodium,indometacin,phenylbutazone and chlorpheniramine in cosmetics by ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS).Four kinds of cosmetics such as cream,facial mask,gel and spray were selected as the representative matrixes.The sample pretreatment conditions were optimized in detail.The cosmetic samples were firstly extracted with acetonitrile by ultrasonic-assisted liquid-liquid extraction,then separated on an ACQUITY UPLC BEH C,18, column(2.1 mm × 100 mm,1.7 μm) by gradient elution,with acetonitrile and water both containing 5 mmol/L ammonium acetate as the mobile phases at a flow rate of 0.3 mL/min and an injection volume of 10 μL,and finally detected by tandem mass spectrometry under multiple reaction monitoring(MRM) scanning mode.Retention times and charge-mass ratio of the compounds(parent ion and two daughter ions) were used for qualitative analysis.Quantitative analyses were carried out by the matrix standard curves using the peak areas of the daughter ions with higher intensity.The results showed that there were good linear relationships for six compounds in the range of 5-200 μg/L with their correlation coefficients(,r,) larger than 0.99.The limits of detection(LOD) and limits of quantitation(LOQ) of the method were 0.15 μg/g and 0.50 μg/g,respectively.The recoveries at three spiked levels for the six components in four matrixes ranged from 75.0% to 120%,with intra-day relative standard deviations(RSD) not more than 7.9% and inter-day RSD no more than 9.7%.With the advantages of simplicity,high sensitivity and accuracy,this method is suitable for the determination of analgesic chemical components in various cosmetics substrates,and it also provides a technical support for the safety supervision of cosmetics.
超高效液相色谱-串联质谱化妆品镇痛药物
ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)cosmeticsanalgesicdrugs
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