摘要
该研究建立了高效液相色谱-二极管阵列检测器法测定洋葱中的硫化丙烯和烯丙基硫醚方法。样品中加入丁硫醇后经乙腈提取,用无水硫酸钠吸收多余的水分后离心,用Thermo Hypersil GOLD液相色谱柱(150 mm×4.6 mm,5μm),以乙腈和水为流动相,流速为1.0 mL/min,柱温为35℃,进样量为10μL,高效液相色谱-二极管阵列检测器检测范围为190~400 nm,检测波长为200 nm。硫化丙烯和烯丙基硫醚在1~100μg/mL质量浓度内线性相关系数R为0.99997~0.99998,方法检出限为0.5 mg/kg,定量限为1.5 mg/kg,5、10、15μg/mL 3个浓度加标水平的回收率为96%~103%,相对标准偏差分别为0.28%~0.49%。该方法前处理简单,科学性、准确性、重现性、精密性好,适用于洋葱中硫化丙烯和烯丙基硫醚分析检测。
A method for the determination of propylene sulfide and diallyl sulfide in onion by high-performance liquid chromatography with a diode array detector was established.After adding butyl mercaptan to the sample,it was extracted with acetonitrile and excess water was absorbed with anhydrous sodium sulfate before centrifugation,Thermo Hypersil GOLD liquid chromatography column(150 mm×4.6 mm,5μm)was used,with acetonitrile and water as the mobile phase,a flow rate of 1.0 mL/min,column temperature of 35℃,and injection volume of 10μL.The detection range of the diode array detector was 190-400 nm,and the detection wavelength was 200 nm.The linear correlation coefficient R in 1-100μg/mL of the propylene sulfide and diallyl sulfide concentration was 0.99997-0.99998 and the detection limit of propylene sulfide and diallyl sulfide was 0.50 mg/kg,and the quantification limit of propylene sulfide and diallyl sulfide was 1.50 mg/kg.The recovery rate of the three concentration spiking levels of 5μg/mL,10μg/mL,and 15μg/mL was 96%-103%and the relative standard deviations were 0.28%-0.49%.The method has simple pretreatment,good scientificity,accuracy,reproducibility and precision,and is suitable for the analysis and detection of propylene sulfide and diallyl sulfide in onion.
作者
任兴权
赵俊
刘盼
霍文清
REN Xingquan;ZHAO Jun;LIU Pan;HUO Wenqing(Jiuquan Food Inspection and Testing Center,Jiuquan 735000,China)
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2024年第6期241-246,共6页
Food and Fermentation Industries
基金
甘肃省自然科学基金(21 JR7RF888)。
关键词
高效液相色谱
二极管阵列检测器
洋葱
硫化丙烯
烯丙基硫醚
high-performance liquid chromatography
diode array detector
onion
propylene sulfide
diallyl sulfide
