分散固相萃取结合UPLC-MS/MS检测烘焙咖啡中19种化学成分OA

A detection method based on dispersive solid phase extraction coupled with ultra-perfor‑mance liquid chromatography-tandem mass spectrometry(d-SPE/UPLC-MS/MS)was established for the simultaneous determination of 19 chemical components in roasted coffee.This method compared the effects of solvent type,feed-to-solvent ratio,solvent pH value,ascorbic acid concentration,ul‑trasonication time,and the type and amount of adsorbent used as the packing material for sample pu‑rification.The optimal experimental conditions selected were a solid-liquid ratio of 1∶10,with 70%ethanol aqueous solution at pH 2 as the extraction solvent,the ascorbic acid concentration was 5 mg/mL,ultrasound time of 60 minutes,and purification packing consisting of 60 mg octadecylsilane(C18),30 mg diatomaceous earth(DE),and 20 mg primary secondary amine(PSA).Using a 0.01%formic acid aqueous solution and a 0.01%formic acid methanol as the mobile phase,separation was achieved within 6 minutes using a Kinetex PFP column(100 mm×3 mm,2.6 μm).The validation re‑sults demonstrated an excellent linear relationship for all 19 compounds across the concentration range of 0.2-5 000 μg/L(r²>0.995).The verification results show that,with the exception of malic acid(LOD is 100 μg/L;LOQ is 200 μg/L),the limits of detection(LODs)and limits of quantifica‑tion(LOQs)for the other 18 compounds range from 0.1 to 20 μg/L and 0.2 to 50 μg/L,respective‑ly.The recoveries for spiked samples at three concentration levels ranged from 73.2%to 111%,with relative standard deviations ranging from 1.4%to 11%.This method was applied to the analysis of 21 batches coffee samples from Yunnan with different processing combinations(variety×processing meth‑od×roasting degree),and combined with principal component analysis(PCA)for statistical analysis.The results indicated that among the measured chemical components,Yellow Bourbon has the high‑est total sum,in addition,the content of the majority of phenolic acids contained in coffee beans tends to decrease gradually as the degree of roasting increases.For the part of flavonoids,which mainly include catechin and epicatechin,tends to increase steadily with the degree of roasting.This research not only provides a specific technical method for detecting chemical components in Yunnan coffee but also offers reliable theoretical support for the processing procedures and production practic‑es of high-quality coffee.