醋酸酐衍生-气相色谱-质谱联用测定葡萄酒中的糖醇

引用本文: 周洪斌, 熊治渝, 余杨, 万荣, 李平, 沈波. 醋酸酐衍生-气相色谱-质谱联用测定葡萄酒中的糖醇[J]. 色谱, 2013, 31(8): 786-790. doi: 10.3724/SP.J.1123.2013.01005 shu

Citation: ZHOU Hongbin, XIONG Zhiyu, YU Yang, WAN Rong, LI Ping, SHEN Bo. Determination of alditols in wine by gas chromatography-mass spectrometry after acetate derivatization[J]. Chinese Journal of Chromatography, 2013, 31(8): 786-790. doi: 10.3724/SP.J.1123.2013.01005 shu

醋酸酐衍生-气相色谱-质谱联用测定葡萄酒中的糖醇

周洪斌 ^{1,
,} ,
熊治渝 ^2, ,
余杨 ^1, ,
万荣 ^1, ,
李平 ^1, ,
沈波 ^1,

通讯作者: 周洪斌

基金项目:
国家质量监督检验检疫总局公益性科研项目(2012424012-3). (2012424012-3)

摘要: 建立了先采用醋酸酐衍生然后用气相色谱-质谱联用仪检测葡萄酒中糖醇的方法。在葡萄酒中加入吡啶涡旋混合均匀,以5000 r/min (4℃)离心10 min。取上清液过有机滤膜,加入吡啶、醋酸酐衍生。加无水硫酸钠吸水后,经DB-5MS毛细管气相色谱柱分离,在选择离子监测(SIM)模式下进行检测。各目标物在0.019~1.25 mg/L (乳糖醇在0.039~2.50 mg/L)范围内线性关系良好,相关系数(r²)均大于0.99。赤藓糖醇、木糖醇、甘露糖醇、山梨糖醇、半乳糖醇和乳糖醇的定量限(信噪比(S/N)=10)分别为0.17、0.29、0.43、0.46、0.47和2.88 mg/L;检出限(S/N=3)分别为0.05、0.08、0.13、0.14、0.14和1.38 mg/L。在40 mg/L和80 mg/L加标水平下,6种糖醇在葡萄酒基质中的回收率为80.15%~108.75%,相对标准偏差(RSD)为2.16%~6.97%。该方法的灵敏度、准确度和精密度均符合相关的技术要求,适合于葡萄酒中糖醇含量的快速检测。

关键词:

衍生
/ 气相色谱-质谱
/ 糖醇
/ 葡萄酒

English

Determination of alditols in wine by gas chromatography-mass spectrometry after acetate derivatization

ZHOU Hongbin ^{1,
,} ,
XIONG Zhiyu ^2, ,
YU Yang ^1, ,
WAN Rong ^1, ,
LI Ping ^1, ,
SHEN Bo ^1,

1.
1. State Key Laboratory of Food Additive and Condiment Testing, Zhenjiang 212008, China;

Corresponding author: 周洪斌

Received Date: 05 January 2013
Fund Project:
国家质量监督检验检疫总局公益性科研项目(2012424012-3).

Abstract: The acetate derivatization of alditols for determining alditol level in wine by gas chromatography (GC)-mass spectrometry (MS) has been developed. The wine sample was mixed with pyridine and centrifuged at 5000 r/min at the temperature of 4℃ for 10 min. After filtration with organic phase membrane, the supernatant was derivatized with acetic anhydride, and then dehydrated with anhydrous sodium sulfate. The GC separation was performed on a DB-5MS capillary column. The alditols were determined by MS in selected ion monitoring (SIM) mode and quantified by external standard method. The calibration curves showed good linearities in the range of 0.019-1.25 mg/L except for lactitol (0.039-2.50 mg/L) with the correlation coefficients greater than 0.99. The limits of quantification (S/N=10) of erythritol, xylitol, D-mannitol, sorbitol, galactitol and lactitol were 0.17, 0.29, 0.43, 0.46, 0.47 and 2.88 mg/L respectively. The limits of detection (S/N=3) were 0.05, 0.08, 0.13, 0.14, 0.14 and 1.38 mg/L respectively. The recoveries of alditols spiked in the wine at two levels of 40 mg/L and 80 mg/L were ranged from 80.15% to 108.75% with the relative standard deviations (RSDs) of 2.16%-6.97%. The sensitivity, accuracy and precision of the method can meet the technical standard. The method can be applied to the rapid determination of alditols in wine.

Key words:

derivatization
/ gas chromatography-mass spectrometry (GC-MS)
/ alditol
/ wine

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沈阳化工大学材料科学与工程学院沈阳 110142

醋酸酐衍生-气相色谱-质谱联用测定葡萄酒中的糖醇

通讯作者: 周洪斌

English

Determination of alditols in wine by gas chromatography-mass spectrometry after acetate derivatization

Corresponding author: 周洪斌

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

醋酸酐衍生-气相色谱-质谱联用测定葡萄酒中的糖醇

通讯作者: 周洪斌

English

Determination of alditols in wine by gas chromatography-mass spectrometry after acetate derivatization

Corresponding author: 周洪斌

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

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CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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