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硅烷化衍生-气相色谱-质谱联用法测定橙汁粉中维生素C
引用本文:崔庆新,宋翠,王方. 硅烷化衍生-气相色谱-质谱联用法测定橙汁粉中维生素C[J]. 理化检验(化学分册), 2010, 0(4)
作者姓名:崔庆新  宋翠  王方
作者单位:聊城大学化学化工学院;聊城市产品质量监督检验所;
摘    要:橙汁粉样品用N,N-二甲基甲酰胺提取,并离心分离,所得上清液中抗坏血酸与六甲基二硅氨烷和三甲基氯硅烷进行衍生反应,产物用正庚烷萃取。萃取液加入棕榈酸甲酯作为内标,供气相色谱-质谱分析。在气相色谱分离中用HP-5MS毛细管柱(30 m×250μm,0.25μm)为固定相,在质谱测定中采用全扫描模式。硅烷化抗坏血酸标准与内标峰面积的比值与硅烷化抗坏血酸的质量在1.0~5.0 mg范围内呈线性关系。方法用于橙汁粉样品中维生素C的测定,橙汁粉中维生素C的平均质量分数(n=6)为0.195 4%,回收率在92.3%~98.5%之间。

关 键 词:气相色谱-质谱联用法  衍生化  橙汁粉  抗坏血酸(维生素C)  

GC-MS Determination of Vitamin C in Orange Juice Powder with Derivatization of Silanization
CUI Qing-xin,SONG Cui,WANG Fang. GC-MS Determination of Vitamin C in Orange Juice Powder with Derivatization of Silanization[J]. Physical Testing and Chemical Analysis Part B:Chemical Analgsis, 2010, 0(4)
Authors:CUI Qing-xin  SONG Cui  WANG Fang
Affiliation:1.School of Chemeistry and Chemeical Engineering/a>;Liaocheng Uneiweisity/a>;Liaocheng 252059/a>;China/a>;2.Liaocheng Supervison and Inspection Institute of Product Quality/a>;Liaocheng 252000/a>;China
Abstract:The powder sample of orange juice was extracted with DMF and separated by centrifugation. Ascorbic acid in the supernatant was derivatized with hexamethyldisilazane and trimethylchlorosilane,and the derivatized product were extracted with n-heptane.The extract was used for GC-MS analysis after adding methyl hexadecanoate(or methyl palmitate) as internal standard.The HP-5MS capillary column was used for GC separation and the full-scanning mode was adopted in MS determination.Linear relationship between value...
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