CN110531005A - 一种检测山地玫瑰花香气成分的方法 - Google Patents
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Abstract
本发明公开了一种检测山地玫瑰花香气成分的方法,该方法是手动进样‑固相微萃取结合嗅闻检测‑气相色谱质谱法,即SPME‑GC‑O‑MS方法;具体的做法包括:第一步,制作样品;第二步,样品前处理;第三步,固相微萃取;第四步,气相色谱检测;第五步,嗅闻检测;第六步,定性分析;第七步,定量分析;第八步,香气成分的评价。本发明的方法首次提供了一种能够对山地玫瑰花中特征挥发性成分进行相对准确的检测方法,从而明确测定山地玫瑰花的香气即挥发性成分,为山地玫瑰花的开发应用提供理论依据;适用于生地玫瑰花的种植与加工。
Description
技术领域
本发明涉及测试气体成分的方法,进一步而言,涉及检测玫瑰花香气成分的方法。
背景技术
玫瑰是蔷薇科蔷薇属的多年生常绿或落叶丛生灌木,原产于中国。玫瑰花(Rosa rugosa)蕾香嫩、润泽、性温、味甘微苦。玫瑰花化学成分多样,主要包含挥发油、黄酮、鞣质、多糖、氨基酸等,具有药用价值、食用价值、观赏价值以及临床应用,如玫瑰花具有抗血栓,调血脂抗衰老等作用,以及玫瑰花在临床上在抑郁、心血管方面的应用。玫瑰花的挥发性成分主要为醇类(如香茅醇、苯乙醇、香叶醇、芳樟醇)、酯类(如乙酸乙酯、乙酸香茅酯、苯乙酸苯乙酯)、酚类(如丁香酚、异丁香酚、)等;据研究,玫瑰花具有抗氧化、抗菌、抗炎、抗肿瘤、降血脂等功效,比如用玫瑰花制成的精油中所含的松油醇、香叶醇、丁香酚等成分,均有较好的抗氧化活性,丁香油酚可通过氧化破坏、膜改变、核酸损伤等途径增加乳腺癌MCF-7细胞对化疗的敏感性;玫瑰花中含有的芳香族物质能够刺激人的呼吸中枢, 调节人的神经系统, 从而促进人体吸进氧气, 排除二氧化碳, 大脑因得到充分的氧气供应, 产生旺盛的精力, 思维清晰敏捷等, 心理高级认知功能得到提高。
目前, 研究风味物质常用的技术有:气相色谱-质谱联用 (gas chromatography-mass spectrometry, GC-MS) 、气相色谱-嗅闻 (GC-olfactometry, GC-O) 和电子鼻分析等。GC-MS具有高分离能力、高选择性、高灵敏度的特点, 同时能够分析物质的分子质量与结构信息。但其不能对所检测到的化合物进行气味归类。嗅闻仪类似于人的鼻子, 可以分析气流中的香味活性。GC-O-MS(固相微萃取结合嗅闻检测 气相色谱质谱法)联用技术是结合二者的特性, 既能鉴定物质结构还可有效地鉴别食品中关键的气味活性成分, 从而了解各化合物对食品气味的贡献程度。这一技术现已应用于酒类、肉类以及饮料等分析检测。
香气是食用玫瑰品质的关键评价指标,决定着其核心产品玫瑰精油的构成、品质及得率。目前,关于研究玫瑰花挥发性的报道有很多,而对山地玫瑰花挥发性成分---香气的研究报道寥寥无几。
中国专利数据库中涉及检测玫瑰花相关的专利申请件仅3件,即2008100583550号《通过颜色识别玫瑰花干燥质量的检测方法》、2012105686102号《一种检测玫瑰花精油含量的方法》、201910029220X号《一种固相微萃取检测玫瑰花制品中精油含量的检测方法》,这些专利技术尚不能检测山地玫瑰花的香气成分。
发明内容
本发明旨在提供一种检测山地玫瑰花香气成分的方法,以明确山地玫瑰花的挥发性成分,为山地玫瑰花的开发应用提供依据。
发明人提供检测山地玫瑰花香气成分的方法,是手动进样-固相微萃取结合嗅闻检测-气相色谱质谱法,即SPME-GC-O-MS方法;具体的做法包括:
第一步,制作样品
取经过干燥的净玫瑰花,用专用袋子密封,粉碎、磨细成玫瑰花粉末;分别随机定量称取玫瑰花粉末置于样品瓶中,备用;
第二步,样品前处理
将第一步的样品置于顶空瓶中,按比列加入去离子水,再用带有橡胶隔垫的瓶盖密封,放入数显恒温水浴锅中,平衡,然后将微萃取头插入顶空瓶中,萃取,然后解析,处理后的样品备用;
第三步,固相微萃取
对样品加热升温;然后在250℃、载气He、流速1mL/min的条件下,用HP-TNNOWAX色谱柱进行固相微萃取,得到萃取物备用;
第四步,气相色谱检测
对上一步的萃取物进行气相色谱的全扫描,得到色谱图;
第五步,嗅闻检测
用ODP3嗅闻仪对样品进行嗅闻检测;
第六步,定性分析:
采用保留指数、MS和嗅闻3种方法进行结构鉴定;
第七步,定量分析
采用面积归一化法对各化合物的相对含量进行定量分析;
第八步,香气成分的评价
由4位评价员在嗅闻仪检测口记录得到香气成分的保留时间、香味特征和强度,强度分为五个等级打分,并尽可能地对所感觉到的香味进行描述,与文献报道的化合物香气特征进行对比,得出评价结论。
上述方法的第一步中,所述随机定量称取玫瑰花粉末置于样品瓶中通常是称量玫瑰花2g置于20mL样品瓶中,样品重复18次。
上述方法的第二步中,所述按比例加入去离子水的比例为样品∶去离子水为1∶3;所述恒温水浴锅温度为60℃,所述平衡时间为20min;所述微萃取头为50/30μmDVB/CAR/PDMS微萃取头,萃取时间为30min,解析时间为5min。
上述方法的第三步中,所述对样品加热升温的过程是:起始温度50℃,保持1min,以5℃/min速率升至200℃,保持5min,以10℃/min速率升至240℃,保持3min;最后达到250℃。
上述方法的第四步中,所述气相色谱全扫描的控制条件为离子源温度230℃、MS四极杆温度150℃、质量扫描范围m/z35~500、质谱库为NIST MS Search2.2。
上述方法的第五步中,所述嗅闻检测的条件是:传输线温度200℃、载气为N2、接口温度为180℃。
上述方法的第六步中,所述MS是通过人工解析并使用计算机检索质谱库NIST MSSearch2.2进行对照鉴定。
上述方法的第八步中,所述强度分为的五个等级是:0表示无、1表示微弱、2表示中等、3表示较明显、4表示非常明显。
本发明的方法首次提供了一种能够对山地玫瑰花中特征挥发性成分进行相对准确的检测方法,从而明确测定山地玫瑰花的香气即挥发性成分,为山地玫瑰花的开发应用提供理论依据;适用于生地玫瑰花的种植与加工。
附图说明
图1为玫瑰花总离子流色谱图。
具体实施方式
实施例 2018年11月6日对贵州省贞丰县精品农业综合开发有限公司提供的干玫瑰花香气成分进行检测
1.采样
从贞丰县精品农业综合开发有限公司购买已经处理好的干玫瑰花,并用玫瑰花专用袋子密封带回实验室,通过机器加工,制作成玫瑰花粉末;分别随机称量玫瑰花2g置于20mL样品瓶中,样品重复18次。
2.样品前处理
准确称取玫瑰花2g于20ml顶空瓶中,按1∶3比列加入6ml去离子水,再用带有橡胶隔垫的瓶盖密封,放入数显恒温水浴锅中,在60℃温度条件下平衡20min,然后将50/30μmDVB/CAR/PDMS微萃取头插入顶空瓶中距液面2cm处,萃取30min,解析5min,待GC-O-MS分析。
3. 固相微萃取
条件:进样口温度250℃;载气He;流速1mL/min;HP-TNNOWAX色谱柱(30m×250um×0.25um);程序升温:起始温度50℃,保持1min,以5℃/min速率升至200℃,保持5min,以10℃/min速率升至240℃,保持3min。
4. 气相色谱检测
条件:离子源温度230℃;MS四极杆温度150℃;质量扫描范围m/z35~500;质谱库为NISTMS Search2.2;扫描模式为全扫描。
5. 嗅闻检测
条件:传输线温度200℃,载气为N2,接口温度为180℃;用ODP3嗅闻仪进行检测。
6. 定性分析
采用保留指数、MS和嗅闻3种方法进行结构鉴定;MS是通过人工解析并使用计算机检索质谱库NIST MS Search2.2进行对照鉴定。
7.定量分析
采用面积归一化法对各化合物的相对含量进行定量分析。
8.香气成分的评价
由4位评价员在嗅闻仪检测口记录得到香气成分的保留时间、香味特征和强度,强度分为0、1、2、3、4五个等级,根据0表示无、1表示微弱、2表示中等、3表示较明显、4表示非常明显来打分,并尽可能地对所感觉到的香味进行描述,与文献报道的化合物香气特征进行对比。
检测结果:通过实验以山地玫瑰花作为研究对象,结果表明,从玫瑰花中共检测出15种化合物,其中脂类化合物4种占23.36%,醇类化合物4种占34.97%,酚类化合物3种占32.28%,其余化合物4种占9.39%;其玫瑰花的主要挥发性成分以脂类、醇类和酚类为主,占总化合物的90.61%,其余化合物作为玫瑰花的辅助成分;与钱宗耀等人实验结果鉴定出16种化学成分相比较,发现与山地玫瑰花中的化合物存在差别。
在GC-MS的基础上,联用嗅闻仪检测,实验结果得到贵州山地玫瑰花的特征香气成分为5种,分别为甲基丁香酚、苯乙醇、甲酸香草脂、香叶醇、异丁香酚,这些成分为玫瑰花的特征挥发性成分作出主要贡献,与苗潇潇[9]等人关于玫瑰花香气成分的实验结果有差异;其中以甲酸香草脂、异丁香酚的香气强度最强,分别带有玫瑰花香气和丁香香气,可以应用在饮料、香水、精油的制作中。
本实验通过对山地玫瑰花特征挥发性成分的检测,为下一步研究山地玫瑰花的应用奠定基础,为山地玫瑰花的发展提供一定的理论依据。
Claims (8)
1.一种检测山地玫瑰花香气成分的方法,其特征在于:该方法是手动进样-固相微萃取结合嗅闻检测-气相色谱质谱法,即SPME-GC-O-MS方法;具体的做法包括:
第一步,制作样品
取经过干燥的净玫瑰花,用专用袋子密封,粉碎、磨细成玫瑰花粉末;分别随机定量称取玫瑰花粉末置于样品瓶中,备用;
第二步,样品前处理
将第一步的样品置于顶空瓶中,按比列加入去离子水,再用带有橡胶隔垫的瓶盖密封,放入数显恒温水浴锅中,平衡,然后将微萃取头插入顶空瓶中,萃取,然后解析,处理后的样品备用;
第三步,固相微萃取
对样品加热升温;然后在250℃、载气He、流速1mL/min的条件下,用HP-TNNOWAX色谱柱进行固相微萃取,得到萃取物备用;
第四步,气相色谱检测
对上一步的萃取物进行气相色谱的全扫描,得到色谱图;
第五步,嗅闻检测
用ODP3嗅闻仪对样品进行嗅闻检测;
第六步,定性分析:
采用保留指数、MS和嗅闻3种方法进行结构鉴定;
第七步,定量分析
采用面积归一化法对各化合物的相对含量进行定量分析;
第八步,香气成分的评价
由4位评价员在嗅闻仪检测口记录得到香气成分的保留时间、香味特征和强度,强度分为五个等级打分,并尽可能地对所感觉到的香味进行描述,与文献报道的化合物香气特征进行对比,得出评价结论。
2.按照权利要求1所述的方法,其特征在于第一步中,所述随机定量称取玫瑰花粉末置于样品瓶中通常是称量玫瑰花2g置于20mL样品瓶中,样品重复18次。
3.按照权利要求1所述的方法,其特征在于第二步中,所述按比例加入去离子水的质量比例为样品∶去离子水为1∶3;所述恒温水浴锅温度为60℃,所述平衡时间为20min;所述微萃取头为50/30μmDVB/CAR/PDMS微萃取头,萃取时间为30min,解析时间为5min。
4.按照权利要求1所述的方法,其特征在于第三步中,所述对样品加热升温的过程是:起始温度50℃,保持1min,以5℃/min速率升至200℃,保持5min,以10℃/min速率升至240℃,保持3min;最后达到250℃。
5.按照权利要求1所述的方法,其特征在于第四步中,所述气相色谱全扫描的控制条件为离子源温度230℃、MS四极杆温度150℃、质量扫描范围m/z35~500、质谱库为NIST MSSearch2.2。
6.按照权利要求1所述的方法,其特征在于第五步中,所述嗅闻检测的条件是:传输线温度200℃、载气为N2、接口温度为180℃。
7.按照权利要求1所述的方法,其特征在于第六步中,所述MS是通过人工解析并使用计算机检索质谱库NIST MS Search2.2进行对照鉴定。
8.按照权利要求1所述的方法,其特征在于第八步中,所述强度分为的五个等级是:0表示无、1表示微弱、2表示中等、3表示较明显、4表示非常明显。
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