食品科学2024，Vol.45Issue(24)：266-272,7.DOI:10.7506/spkx1002-6630-20240804-026
固相萃取结合超高效液相色谱-串联质谱法快速测定乳粉及液体乳中26种吡咯里西啶生物碱的含量
Rapid Determination of 26 Pyrrolizidine Alkaloids in Milk Power and Liquid Milk by Solid Phase Extraction Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
A method was developed for the simultaneous determination of 26 pyrrolizidine alkaloids(PAs)in milk powder and liquid milk by solid phase extraction(SPE)combined with ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with 5%trichloroacetic acid solution,cleaned up on a polymer cation exchange-solid phase extraction(PCX-SPE)column,separated on an ACQUITY HSS T3 column with gradient elution using a mobile phase consisting of methanol and 0.1%formic acid in water,detected using an electrospray ionization(ESI)in the positive ion mode with multiple reaction monitoring(MRM),and finally quantified by the external standard method.The method validation was performed under optimal conditions.The calibration curves for the 26 PA compounds showed good linearity in the range of 1.0-40 ng/mL with determination coefficients(R2)greater than 0.992.The limits of detection(LOD)and quantification(LOQ)of the developed method were in the range of 0.01-0.33 μg/kg(RS/N=3)and 0.03-1.0 μg/kg(RS/N=10),respectively.Recoveries for blank milk powder and liquid milk spiked at 1×,2×,and 10×LOQ levels ranged from 73.1%to 111.6%with relative standard deviations(RSDs,n=6)of 0.6%-9.8%.In conclusion,this method is simple,efficient,sensitive,accurate,and suitable for the determination of the 26 PAs in milk powder and liquid milk.关键词
固相萃取/超高效液相色谱-串联质谱/乳粉和液体乳/吡咯里西啶生物碱Key words
solid phase extraction/ultra-high performance liquid chromatography-tandem mass spectrometry/milk powder and liquid milk/pyrrolizidine alkaloids分类
轻工业引用本文复制引用
陈言凯..固相萃取结合超高效液相色谱-串联质谱法快速测定乳粉及液体乳中26种吡咯里西啶生物碱的含量[J].食品科学,2024,45(24):266-272,7.基金项目
福建省产品质量检验研究院科研项目(KY202220A) （KY202220A）
市场监管总局科技计划资助项目(2021MK054) （2021MK054）
