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固相微萃取-气相色谱法测定全麦酒酿中乙醇含量
Determination of ethanol content in sweet fermented whole wheat by solid phase microextraction-gas chromatography
【摘要】 目的建立顶空固相微萃取-气相色谱法测定全麦酒酿中乙醇含量。方法在10 m L顶空瓶中加入0.1 g经粉碎或者捣碎的样品和5 m L超纯水,加入氯化钠使其质量分数为40%,于磁力搅拌下预平衡5 min,插入羟基硅油/二乙烯基苯萃取头在50℃萃取10 min,拔出萃取头进入气相色谱仪分析。结果乙醇在100~200000μg/g范围内呈现很好的线性关系,线性相关系数r~2为0.999;方法的检测限为11.92μg/g,在200、2000、20000μg/g 3个加标水平上的回收率均在96.51%~103.48%之间,相对标准偏差小于8.91%。结论该方法操作简便快速,样品用量少,灵敏度高,结果准确,重现性好,适合全麦酒酿等多种酒酿中乙醇含量的测定。
【Abstract】 Objective To establish a method for determination of ethanol content in sweet fermented whole wheat by headspace solid phase microextraction-gas chromatography(HS-SPME-GC). Methods A portion of 0.1 g smashed or mashed sample was diluted with 5 m L of ultrapure water in a 10 m L headspace vial, and then sodium chloride was added to get a concentration of 40%(W:V). The mixture was incubated at 50 ℃ for 5 min with magnetic stirring. A hydroxy-terminated silicone oil/divinyl benzene fiber was inserted and kept extraction for 10 min at 50 ℃. After extraction, the fiber was transferred to the GC injection port for desorption. Results Ethanol was linear in the range of 100~200000 μg/g with correlation coefficient(r~2) of 0.999. The limit of detection was 11.92 μg/g. The recoveries of ethanol were 96.51%~103.48% when spiked at levels of 200, 2000 and 20000 μg/g with the relative standard deviations less than 8.91%. Conclusion The proposed method has the advantages such as simple operation, rapid determination, less sample consumption, high sensitivity, good accuracy and repeatability, which is suitable for determination of ethanol in many kinds of sweet fermented grains.
【Key words】 ethanol; headspace solid phase microextraction; gas chromatography; sweet fermented whole wheat;
- 【文献出处】 食品安全质量检测学报 ,Journal of Food Safety & Quality , 编辑部邮箱 ,2017年04期
- 【分类号】O657.71;TS261.7
- 【被引频次】5
- 【下载频次】244