去屑洗发露中羟吡啶酮的高效液相色谱法检测及质谱确证  

Determination of Hydroxypyridinone in Shampoo by High Performance Liquid Chromatography and Its Confirmation by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：聂明霞 汪毅 梁文耀 贾芳 李露 夏泽敏 陈彦君 谭建华 NIE Ming-xia;WANG Yi;LIANG Wen-yao;JIA Fang;LI Lu;XIA Ze-min;CHEN Yan-jun;TAN Jian-hua(National Quality Supervision and Testing Center for Cosmetics(Guangzhou),Guangzhou Quality Supervision and Testing Institute,Guangzhou 511447,China)

机构地区：[1]广州质量监督检测研究院,国家化妆品质量检验检测中心,广东广州511447

出　　处：《分析测试学报》2023年第1期96-100,106,共6页Journal of Instrumental Analysis

摘　　要：该文建立了去屑洗发露中羟吡啶酮的高效液相色谱法(HPLC)测定及其质谱确证方法。样品采用乙腈涡旋超声提取,以950 mL乙腈+50 mL 400 mmol/L草酸溶液作为流动相,经Waters Atlantis Hilic(4.6 mm×250 mm×5μm)色谱柱分离,用二极管阵列检测器(DAD)进行检测。采用硫酸二甲酯对羟吡啶酮衍生化,以正离子多反应监测模式(MRM)进行质谱确证。结果表明,羟吡啶酮在1.0~100.0 mg/L范围内线性关系良好,相关系数(r)为0.999,方法检出限和定量下限分别为8.0μg/g和20.0μg/g,加标回收率为91.8%~96.7%,相对标准偏差(RSD)为1.3%~3.7%。该方法快速、高效、准确,适用于洗发露及吡硫鎓锌原料中羟吡啶酮的测定。使用液相色谱及傅里叶变换红外光谱对羟吡啶酮及其互变异构体2-羟基吡啶-N-氧化物进行了比较,并阐明了洗发露中禁用原料羟吡啶酮的可能来源。A high performance liquid chromatography(HPLC) and mass spectrometry method was established for the determination and confirmation of hydroxypyridinone in dandruff shampoo. The samples were extracted with acetonitrile,then separated on a Waters Atlantis Hilic(4. 6 mm × 250 mm × 5 μm) column with a mixed solution of 95% acetonitrile and 5% 400 mmol/L oxalic acid as the mobile phase,and detected by HPLC.Mass spectrometry confirmation on hydroxypyridone in positive multiple reaction monitoring(MRM) mode after derivatization of hydroxypyridone with dimethyl sulfate. Results showed that there were good linear relationships for the analytes in the range of 1. 0-100. 0 mg/L,with correlation coefficients(r) of 0. 999.The limits of detection(LODs) and limits of quantitation(LOQs) for hydroxypyridone were 8. 0 μg/g and 20. 0 μg/g,respectively.The spiked recoveries ranged from 91. 8% to 96. 7%,with RSDs of 1. 3%-3. 7%.The method is rapid,efficient and accurate,and it could be applied to the determination of hydroxypyridone in shampoo and zinc pyrithione.In this paper,a series of comparisons were carried out by liquid chromatography and infrared spectroscopy with respect to hydroxypyridone and its tautomer,2-hydroxypyridine-N-oxide.In addition,the possible source of hydroxypyridinone,a prohibited raw material in shampoo,was clarified.

关 键 词：羟吡啶酮 2-羟基吡啶-N-氧化物 去屑剂 高效液相色谱法 液相色谱-串联质谱法 

分 类 号：O657.7[理学—分析化学] O657.3[理学—化学]