CAJ | 학술논문

目的：比较液液萃取法、固相萃取法和分散式固相萃取法作为预处理方法对葡萄酒中的氨基甲酸乙酯的处理效率。方法葡萄酒样品中的氨基甲酸乙酯分别用二氯甲烷进行液液萃取，用氨基甲酸乙酯专用柱进行固相萃取，用乙腈、石墨化炭黑和N-丙基乙二胺进行分散式固相萃取，再以气相色谱-质谱联用仪测定其含量。结果3种预处理方法的平均回收率均在70%~110%之间，相对标准偏差(n=5)均小于6%。液液萃取法处理单个样品成本小于5元，富集倍数可达5倍，可用于低含量样品的预处理和进出口企业的产品合规性检测；固相萃取法操作简便，每人每工作日可处理40个样品，可用于企业的高通量检测；分散式固相萃取法成本适中、回收率最佳、综合预处理效率高，一次预处理可同时检测葡萄酒中农药残留和氨基甲酸乙酯含量，适用于葡萄酒中多种危害物质的筛查。结论三种方法各具优势，综合考虑处理效率和实验成本，分散式固相萃取法更适合葡萄酒生产企业的日常应用。该方法已用于葡萄酒中氨基甲酸乙酯的含量测定。
목적：비교액액췌취법、고상췌취법화분산식고상췌취법작위예처리방법대포도주중적안기갑산을지적처리효솔。방법포도주양품중적안기갑산을지분별용이록갑완진행액액췌취，용안기갑산을지전용주진행고상췌취，용을정、석묵화탄흑화N-병기을이알진행분산식고상췌취，재이기상색보-질보련용의측정기함량。결과3충예처리방법적평균회수솔균재70%~110%지간，상대표준편차(n=5)균소우6%。액액췌취법처리단개양품성본소우5원，부집배수가체5배，가용우저함량양품적예처리화진출구기업적산품합규성검측；고상췌취법조작간편，매인매공작일가처리40개양품，가용우기업적고통량검측；분산식고상췌취법성본괄중、회수솔최가、종합예처리효솔고，일차예처리가동시검측포도주중농약잔류화안기갑산을지함량，괄용우포도주중다충위해물질적사사。결론삼충방법각구우세，종합고필처리효솔화실험성본，분산식고상췌취법경괄합포도주생산기업적일상응용。해방법이용우포도주중안기갑산을지적함량측정。
Objective To compare the preconditioning efficiencies of ethyl carbamate in wine by liquid-liquid extraction (LLE), solid phase extraction (SPE) and dispersive solid phase extraction (d-SPE). MethodThree methods of LLE with dichloromethane, SPE with Cleanert EC column and d-SPE with acetonitrile, graphitized carbon and primary secondary amine were separately used to extract the ethyl carbamate of the wine samples, which was analyzed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode.Result The spiked recoveries at 3 levels of these methods were in the range of 70%~110% and the relative standard deviations (n=5) were less than 6%, indicating that those methods had a good accuracy and precision. Since it was low-cost and had a high enrichment efficiency, LLE was suitable for pretreatment of samples with trace amount and could meet the requirements of compliance detection in import and export manufacturers. SPE was more appropriate for high through-put determination due to convenience and fast speed. d-SPE could be well applied to various hazard substances screening, because it was mid-cost, best recovery and high comprehensive efficiency.Conclusion In consideration of the pretreatment efficiency and cost, d-SPE was more suitable for the daily quality control inspection in wine manufacturers. d-SPE coupled with GC-MS had been applied to determination of ethyl carbamate in wine.