CN106248827B - 一种2,4-癸二烯醛的提取及检测方法 - Google Patents
一种2,4-癸二烯醛的提取及检测方法 Download PDFInfo
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Abstract
本发明涉及一种2,4‑癸二烯醛的提取及检测方法,本发明提取方法包括如下步骤:准确称取0.2g含有2,4‑癸二烯醛的粉末微胶囊并置于10mL的离心管中,后用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL有机溶剂,超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过膜(0.22um的有机滤膜),即为待测液。本发明方法简单,误差小。
Description
技术领域
本发明涉及一种检测方法,特别涉及一种测定2,4-癸二烯醛的方法。
背景技术
2,4-癸二烯醛是种黄色液体,密度稍稍大于水,沸点104℃,不溶于水,易溶于酒精和大多数非挥发性油。具有强烈的鸡香和鸡油的香气特征,国标规定其为允许使用的食品用香料,主要用于配置鸡肉香精中。
2,4-癸二烯醛不仅是鸡肉油状香精的主要成分,且是呈现强烈鸡脂风味主要特征的物质。因此,可作为测定鸡肉香精微胶囊包埋率的一个标志物,而目前未见有关于从微胶囊中提取2,4-癸二烯醛的方法。
发明内容
本发明的目的是提供一种2,4-癸二烯醛的提取及分析检测方法。
本发明采用的技术方案为:
本发明提供了一种2,4-癸二烯醛的提取方法,该方法包括如下步骤:
准确称取0.2g含有2,4-癸二烯醛的粉末微胶囊并置于10mL的离心管中,后用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL有机溶剂,超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过膜(0.22um的有机滤膜),即为待测液。
优选地,所述的有机溶剂为正己烷、石油醚、氯仿或***。更优选为***。
本发明还提供了一种2,4-癸二烯醛的分析检测方法,该方法包括如下步骤:
(1)2,4-癸二烯醛的提取:
准确称取0.2g含有2,4-癸二烯醛的粉末微胶囊并置于10mL的离心管中,后用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL有机溶剂,超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过膜(0.22um的有机滤膜),即为待测液;
(2)2,4-癸二烯醛的GC检测
将步骤(1)中的待测液置于样品瓶中,旋紧密封盖,进行测样,测定条件如下:
Hp-5毛细管柱(60m×0.25mm×0.25μm),进样口温度250℃,载气为高纯(≥99.999%)氦气,载气流速为1.0mL/min,程序升温:起始温度40℃,保持2.0min,10℃/min升至250℃保持10.0min;
EI离子源;电子能量70eV;四级杆温度150℃,接口温度260℃;电子倍增器电压1423V;离子源温度230℃;采用标准方式调谐;选用全扫描模式,质量扫描范围:40~400amu,溶剂延迟10min。
优选地,所述的有机溶剂为正己烷、石油醚、氯仿或***。更优选为***。
本发明所具有的有益效果:
本发明提供一种2,4-癸二烯醛的提取及分析检测方法,本发明方法简单,误差小。
附图说明
图1为2,4-癸二烯醛的标准曲线。
具体实施方式
下面结合具体实施例对本发明作进一步说明,但不限定本发明的保护范围。
实施例1
一种测定香精粉末中2,4-癸二烯醛的方法,包括如下步骤:
(1)2,4-癸二烯醛的提取:
准确称取0.2g含有2,4-癸二烯醛的粉末微胶囊并置于10mL的离心管中,后用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL***超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过膜(0.22um的有机滤膜),即为待测液;(2)2,4-癸二烯醛的GC检测
将步骤(1)中的待测液置于样品瓶中,旋紧密封盖,即可测样,测定条件如下:
Hp-5毛细管柱(60m×0.25mm×0.25μm),进样口温度250℃,载气为高纯(≥99.999%)氦气,载气流速为1.0mL/min,程序升温:起始温度40℃,保持2.0min,10℃/min升至250℃保持10.0min。
EI离子源;电子能量70eV;四级杆温度150℃,接口温度260℃;电子倍增器电压1423V;离子源温度230℃;采用标准方式调谐;选用全扫描模式,质量扫描范围:40~400amu,溶剂延迟10min。
测定不同有机溶剂的回收率:
对比样品制备:
准确称取0.2g含有2,4-癸二烯醛的粉末微胶囊并置于10mL的离心管,并加入0.03g的2,4-癸二烯醛单体,后用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL有机溶剂,超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过膜(0.22um的有机滤膜),即为待测样;
空白对照样品制备:
准确称取0.2g含有2,4-癸二烯醛的粉末微胶囊并置于10mL的离心管,再用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL有机溶剂,超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过膜(0.22um的有机滤膜),即为待测样;
测定结果如下:
当有机溶剂选择***时,结果如下:
不同有机溶剂对于样品中2,4-癸二烯醛的提取率的测定结果如下表所示:
由上表可以看出,***对于微胶囊中的2,4-癸二烯醛的提取率最高,因此可以选择***作为2,4-癸二烯醛的最佳提取溶剂。
标准曲线的制作:
精确称取0.36g2,4-癸二烯醛单体置于10mL离心管中,再用移液管吸取10mL***,将其溶解,用涡旋振荡器振荡2min,即得浓度为36mg/mL的初始标准液,并依次对上述配置好的标准液作不同梯度的稀释,稀释后的浓度依次为:12mg/mL、6mg/mL、2mg/mL、1mg/mL,测定的标准曲线如图1所示。
重复性实验:
样品提取方法如(1)所示,采用气相分析器对同一个制备好的样品连续进样6次,RSD(%)=1.91%。
精密度实验:
同一样品,样品提取方法如(1)所示,重复提取六次,进样测定,RSD(%)=2.23%。稳定性:
对同一份制备好的样品每隔6小时测定一次,测定至30h止,进样测定,RSD(%)=1.32%。
Claims (1)
1.一种2,4-癸二烯醛的分析检测方法,其特征在于:该方法包括如下步骤:
(1)2,4-癸二烯醛的提取:
准确称取0.2g含有2,4-癸二烯醛的粉末微胶囊并置于10mL的离心管中,后用1mL移液管吸取2mL水将其溶解,待溶解后,再加入4mL有机溶剂,超声1min,静置2min待分层,吸取上清液1mL,并加入0.2g无水硫酸钠,静置12h后过0.22μm的有机滤膜,即为待测液;
(2)2,4-癸二烯醛的GC检测
将步骤(1)中的待测液置于样品瓶中,旋紧密封盖,进行测样,测定条件如下:
Hp-5毛细管柱,60m×0.25mm×0.25μm,进样口温度250℃,载气为≥99.999%的高纯氦气,载气流速为1.0mL/min,程序升温:起始温度40℃,保持2.0min,10℃/min升至250℃保持10.0min;
EI离子源;电子能量70eV;四级杆温度150℃,接口温度260℃;电子倍增器电压1423V;离子源温度230℃;采用标准方式调谐;选用全扫描模式,质量扫描范围:40~400amu,溶剂延迟10min;
所述的有机溶剂为***。
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