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

KeyWord:hydroxypyridinone  2-hydroxypyridine-N-oxide  anti-dandruff agent  high performance liquid chromatographic£¨HPLC£©  liquid chromatography£­tandem mass spectrometry£¨LC£­MS/MS£©

Abstract:

      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 ¡Á 250 mm ¡Á 5 ¦Ìm£© 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 ¦Ìg/g and 20.0 ¦Ìg/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.