红外光谱高效液相色谱法鉴定出土酒残留物

Identification and analysis of archaeological wine residue by infrared spectra-high performance liquid chromatography

在前人研究的基础上,建立红外光谱结合高效液相色谱的方法鉴定出土酒器中酒残留物。先采用红外光谱法对酒的种类进行鉴定,之后采用高效液相色谱法对其中的8种有机酸进行定量检测。针对有机酸的化学性质和样品杂质情况,对酒残留物样品进行萃取方法优化,最终以超纯水进行萃取,经振荡、超声、离心和过滤后再进行测定。采用反相C18色谱柱分离,以0. 01mol/L磷酸氢二铵溶液和100%甲醇为流动相进行等度洗脱(98∶2,体积比),在210nm的波长下检测。结果表明,红外光谱法可以对出土酒残留物的种类进行粗判;用高效液相色谱法检测8种有机酸,方法的相对标准偏差(RSD)在0. 55%～1. 31%之间,定量限为0. 22～20. 00ng/m L,线性相关系数(R2)均大于0. 99。采用该方法对榆林走马梁汉墓出土的残留物进行了分析,结果表明其为采用粮食原料酿造的发酵酒残留物。该方法适用于考古出土酒残留物的鉴定和检测。

Infrared spectroscopy is used to identify whether the samples are wine residue,then using high performance liquid chromatography to make quantitative detection for8organic acids in samples.As residue samples have so many impurities,the detection of organic acids should ensure the optimization of the extraction method.This means that the samples have to do ultrapure water extraction,oscillation,ultrasonic dissolution,centrifugation and filtration.Then using reversed-phase C18chromatographic column to make separation,the mobile phases are0.01mol/L diammonium phosphate solution and100%methanol with isocratic elution.Detection is under the wavelength of210nm.Eight kinds of organic acid can be separated and measured by high performance liquid chromatography method,the relative standard deviations(RSD)of this method are between0.55%and1.31%,quantitative limit is0.22~20.00ng/mL,and all of the linear correlation coefficients(R2)are greater than0.99.The result of infrared spectroscopy reveals that all samples belong to wine residue.Six kinds of organic acids in samples have been detected,including lactic acid,tartaric acid which make great significance in interpreting the procedure of ancient wine.In conclusion,this method is simple,high efficient,low cost,easy to promote,which is suitable for the appraisal and detection of wine residue excavated.