Screening of Illicit Oxyphenisatin Substances in Weight-Loss Dietary Supplements by High Performance Liquid Chromatography-in-Source-Fragmentation-Quadrupole Time-of-Flight Mass Spectrometry
10.19756/j.issn.0253-3820.251145
- VernacularTitle:高效液相色谱-源内裂解-四极杆-飞行时间质谱法筛查减肥食品中的酚丁类非法添加物
- Author:
Hong-Fei SHI
1
;
Ke-Yu LIU
;
Bo-Peng XU
;
Cheng-Xin XU
;
Xiu-Qi ZHOU
;
Yi-Fei ZHOU
;
Ming-Xin GUO
Author Information
1. 南京警察学院刑事科学技术学院,南京 210023
- Keywords:
High-resolution mass spectrometry;
Non-targeted screening;
In-source fragmentation;
Illicit adulteration
- From:
Chinese Journal of Analytical Chemistry
2025;53(9):1576-1585,后插1-后插9,封3
- CountryChina
- Language:Chinese
-
Abstract:
By summarizing the mass spectrometric fragmentation patterns of oxyphenisatin substances,an analytical method was established for screening of illegally added oxyphenisatin compounds in weight-loss health foods using high performance liquid chromatography-in-source-fragmentation-quadrupole time-of-flight mass spectrometry(HPLC-ISF-QTOF-MS),along with a quantitative method for 11 kinds of oxyphenisatin compounds.Based on the developed screening method,an oxyphenisatin derivative was discovered in the reference standards,which was tentatively identified as 4-(3-(4-hydroxyphenyl)-2-oxoindolin-3-yl)phenyl acetate and confirmed by MS/MS analysis.The results showed that all 11 kinds of oxyphenisatin compounds had correlation coefficients greater than 0.9971,with limits of detection(LODs)ranging from 0.12 to 0.68 μg/L and limits of quantification(LOQ)from 0.21 to 2.29 μg/L.The LODs for 11 kinds of characteristic ions ranged from 0.45 to 9.11 μg/kg.At spiking levels of 25,50 and 100 μg/kg,the recoveries ranged from 78.9%to 117.3%.The instrumental precision,intra-day method precision and inter-day method precision were 0.23%?1.70%,0.7%?2.4%,and 1.1%?3.3%,respectively.The developed targeted and non-targeted detection method demonstrated high sensitivity,strong stability,rapid analysis,and an expanded screening range for oxyphenisatin substances,and provided robust technical support for regulatory authorities in combating illegal adulteration.
