[Determination of three furfural compounds in coffee and coffee products by gas chromatography-tandem mass spectrometry with internal standard isotope].

Jianguo Wang, Yue Wang, Fang Wang, Hong Chang, Kai Lei, Guofeng Zhang, Yanchun Wang
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Abstract

Objective: To establish a method for the determination of three furfural compounds in coffee and its products by gas chromatography-tandem mass spectrometry.

Methods: The samples were extracted with ethanol water(1∶2, V∶V) solution, ultrasonic with 10% Na_2CO_3 solution for 5 min, purified with 100 mg C_(18), 50 mg Srong Cation exchang(SCX), 150 mg anhydrous MgSO_4, separated by HP-INNOWAX capillary column(30 m×0.25 mm, 0.25 μm), detected by gas chromatography-tandem mass spectrometry, and quantified by isotope internal standard method.

Results: The correlation coefficients(r) of the three furfural compounds were all greater than 0.999, the limits of detection were 0.004-0.011 mg/kg, and the limits of quantitation were 0.013-0.031 mg/kg. The average recoveries were 86.0%-112% and the relative standard deviations were 4.1%-10.6%(n=6), at 3 supplemental levels in 3 different coffee substrates. Nine samples of coffee beans, instant coffee and coffee drinks were tested, and all three components to be tested were detected.

Conclusion: The method is simple, rapid, sensitive, with good accuracy and precision. It is suitable for the determination of three furfural compounds in coffee and its products.

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[气相色谱-内标同位素串联质谱法测定咖啡及咖啡制品中的三种糠醛化合物]。
目的:建立气相色谱-串联质谱法测定咖啡及其制品中3种糠醛化合物的方法。方法:用乙醇水(1∶2,V∶V)溶液提取,10% Na_2CO_3溶液超声提取5 min,用100 mg C_(18)、50 mg强阳离子交换(SCX)、150 mg无水MgSO_4纯化,HP-INNOWAX毛细管柱(30 m×0.25 mm, 0.25 μm)分离,气相色谱-串联质谱法检测,同位素内标法定量。结果:3种糠醛化合物的相关系数(r)均大于0.999,检出限为0.004 ~ 0.011 mg/kg,定量限为0.013 ~ 0.031 mg/kg。在3种不同咖啡基质中添加3种添加水平,平均回收率为86.0% ~ 112%,相对标准偏差为4.1% ~ 10.6%(n=6)。对咖啡豆、速溶咖啡和咖啡饮料等9种样品进行了检测,三种成分均被检测到。结论:该方法简便、快速、灵敏,准确度和精密度好。本法适用于咖啡及其制品中三种糠醛类化合物的测定。
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