CAJ | 학술논문

目的：建立了离子色谱-质谱联用技术测定葡萄酒样品中柠檬酸的分析方法。方法以高容量、强亲水性的IonPac AS20型阴离子交换柱为分析柱, EGC在线产生梯度浓度KOH为淋洗液,淋洗液经捕获柱、抑制器成水后将样品带入质谱检测器。ESI-SIM监测模式监控柠檬酸根离子(m/z=191),并以峰面积进行定量。结果该方法对柠檬酸的检出限(S/N=3)为17.6μg/L,且柠檬酸浓度在50~1000μg/L范围内具有良好的线性,线性相关系数r=0.9992。200μg/L标准溶液重复进样8次,柠檬酸峰面积的相对标准偏差即精密度为0.77%。运用该方法测定市售5种不同品牌葡萄酒样品中柠檬酸的含量,并对样品加标回收,得回收率大于95%。结论该方法可以满足葡萄酒中柠檬酸定量分析的要求,且有效改善了分析的灵敏度和准确性。
목적：건립료리자색보-질보련용기술측정포도주양품중저몽산적분석방법。방법이고용량、강친수성적IonPac AS20형음리자교환주위분석주, EGC재선산생제도농도KOH위림세액,림세액경포획주、억제기성수후장양품대입질보검측기。ESI-SIM감측모식감공저몽산근리자(m/z=191),병이봉면적진행정량。결과해방법대저몽산적검출한(S/N=3)위17.6μg/L,차저몽산농도재50~1000μg/L범위내구유량호적선성,선성상관계수r=0.9992。200μg/L표준용액중복진양8차,저몽산봉면적적상대표준편차즉정밀도위0.77%。운용해방법측정시수5충불동품패포도주양품중저몽산적함량,병대양품가표회수,득회수솔대우95%。결론해방법가이만족포도주중저몽산정량분석적요구,차유효개선료분석적령민도화준학성。
Objective To establish a rapid method for determination of citric acid in wine samples by ion chromatography-electrospray ionization tandem mass spectrometry (IC/ESI-MS) in the negative ESI and se-lected ion monitor (SIM) mode. Methods Citric acid was separated by high capacity and hydroxide selective column IonPac AS20 with KOH eluent generated from EGC. Peak area of citrate ion (m/z=191) was monitored for quantifying. Results The limit of detection was 17.6μg/L for citric acid. A linear calibration was obtained over the range from 50 to 1000μg/L with a correlation coefficient of 0.9992. The relative standard deviation for 8 injections of standard solution (200 μg/L) was 0.77%. This method was applied to detect the citric acid in different kinds of wine samples which were purchased in market, and the rates of recovery were higher than 95%. Conclusion The method could meet the requirements of quantitative analysis of citric acid in wine samples, and also could improve the sensitivity and accuracy of the analysis.