食品科学2026，Vol.47Issue(1)：301-308,8.DOI:10.7506/spkx1002-6630-20250728-216
室温皂化联合气相色谱-四极杆-飞行时间质谱检测肉制品中的胆固醇氧化物
Determination of Cholesterol Oxidation Products in Meat Products by Saponification at Room Temperature Combined with Gas Chromatography-Quadrupole-Time-of-Flight Mass Spectrometry
摘要
Abstract
In view of the diverse forms and unstable properties of cholesterol oxidation products(COPs)in meat products under specific conditions,a sample pretreatment technology,saponification at room temperature,was established for the accurate detection of 9 COPs in meat products by gas chromatography-quadrupole-time-of-flight mass spectrometry(GC-Q-TOF/MS).The results showed that the optimal pre-treatment conditions were extraction with chloroform/methanol(2:1,V/V),saponification at room temperature for 18 h,re-extraction with ethyl acetate/n-hexane(80:20,V/V),and clean-up using an aminopropyl solid-phase extraction(SPE)cartridge.The linear ranges were 0.002–0.5 μg/mL for 7α-hydroxyl cholesterol and 7β-hydroxyl cholesterol,and 0.02–0.5 μg/mL for 5β,6β-epoxide cholesterol,5α,6α-epoxide cholesterol,20α-hydroxy cholesterol,3β,5α,6β-trihydroxy cholesterol,25α-hydroxy cholesterol,7-keto cholesterol and 27α-hydroxy cholesterol.The determination coefficients were≥0.999 0 for all analytes,the limits of detection(LOQ)were 0.000 1–0.001 mg/kg,and the limits of quantitation(LOQ)were 0.000 2–0.002 mg/kg.The method had good accuracy and high precision.The average recoveries from spiked samples were 89.7%–116.1%,with relative standard deviations(RSDs)of less than 8.7%.Compared with high temperature saponification,saponification at room temperature effectively prevented the autoxidation of cholesterol and the degradation of 7-ketocholesterol,and reduced the exogenous introduction and endogenous loss of target substances,thereby enabling the rapid and accurate detection of the 9 COPs.关键词
肉制品/胆固醇氧化物/室温皂化/7-酮基胆固醇/气相色谱-四极杆-飞行时间质谱Key words
meat products/cholesterol oxidation products/saponification at room temperature/7-keto cholesterol/gas chromatography-quadrupole-time-of-flight mass spectrometry分类
轻工纺织引用本文复制引用
李洁,陈倩倩,王艳丽,田其燕,梁秀清,李霞,李新玲,刘艳明,申中兰..室温皂化联合气相色谱-四极杆-飞行时间质谱检测肉制品中的胆固醇氧化物[J].食品科学,2026,47(1):301-308,8.基金项目
国家市场监督管理总局科技计划项目(2022MK072) （2022MK072）
山东省药品监督管理局科研项目(SDNMPAFZLS202401) （SDNMPAFZLS202401）
