CN112051349A - 一种大麦幼苗挥发性成分的检测方法 - Google Patents
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Abstract
本发明涉及植物学分析技术领域，具体是一种检测大麦幼苗中挥发性成分的检测方法，所述的检测方法为顶空固相微萃取和气相色谱－质谱联用法，即HS‑SPME‑GC‑MS。本发明的方法通过对萃取条件和色谱条件进行限定，使待测样品中多种挥发性成分之间完全分离，从而能够准确地同时测定出待测样品中多种挥发性成分的相对含量，其准确性好、灵敏度高、结果稳定，可用于大麦幼苗中挥发性成分的检测，从而明确了大麦幼苗中的挥发性成分，为大麦幼苗的种植加工和开发应用提供理论依据。
Description
技术领域
本发明涉及植物学分析技术领域，具体地说，是一种利用顶空固相微萃取和气相色谱－质谱联用法快速检测大麦幼苗中挥发性成分的方法。
背景技术
大麦(Hordeum vulgare L.)属于禾本科大麦属植物，是世界第四大谷类作物，主要用作啤酒工业原料、畜牧业饲料和食品加工原料。另外，大麦作为我国传统的药食同源植物，还有很好的保健功能，其种子及其麦芽、麦苗均可作药用。麦苗的功效在《本草纲目》中就曾有记载，现代研究表明大麦幼苗中富含多种营养与功能性成分，具有促进睡眠、降糖降脂、抗肿瘤、抗炎、抗氧化等多种生理功能。以大麦幼苗为原料开发的功能型产品也越来越多，例如麦绿素、麦草饮料、青麦酶等。麦绿素等麦苗产品的成功开发提升了麦苗的经济价值。
但是，目前麦苗产品还缺乏专用苗用品种，生产上所使用的仍然是选育的啤酒大麦或饲料大麦品种。国内已有一些麦绿素专用品种筛选的相关研究报道，这些研究主要对大麦幼苗的生物活性成分进行了分析比较。麦苗的品质除了取决于麦苗的生物活性成分含量，还受到挥发性风味物质的影响。
大麦属于低芳香性植物，对其幼苗挥发成分的测定相对较为困难。目前尚未有采用顶空固相微萃取和气相色谱－质谱联用法测定大麦幼苗中挥发性成分的报道，顶空固相微萃取具有集采样、萃取、浓缩与进样为一体，操作简单，灵敏度高，无二次污染等优点。
发明内容
本发明的目的在于提供一种高效、快速的采用顶空固相微萃取(Headspace solidphase micro-extraction，HS-SPME)和气相色谱－质谱(Gas chromatography-massspectrometry，GC-MS)联用法测定大麦幼苗中挥发性成分的方法，所述的方法具有稳定性和可重复性。
目前关于大麦苗挥发性成分的分析鲜见报道。顶空固相微萃取由于集采样、萃取、浓缩与进样为一体，操作简单，灵敏度高，无二次污染等优点，被广泛应用于食品、生物、医药等领域的挥发性成分的分析研究。为明确大麦苗的挥发性成分，筛选主要挥发性物质。本发明以长三角地区主栽大麦品种“花30”和“苏啤3号”为试验材料，采用HS-SPME-GC-MS方法对大麦幼苗挥发性物质进行了分析检测，为大麦幼苗的优质栽培和品质育种提供科学依据。
为了实现上述目的，本发明提供一种大麦幼苗挥发性成分的检测方法，包括以下步骤：
A、样品处理：越冬麦苗长到6-7叶期进行取样，采收的麦苗蒸馏水洗净，吸干水分，在室温条件下5 000r/min匀浆备用；取5g样品于顶空瓶中，封口，待测；
B、萃取条件：萃取头型号，50/30μm DVB/Carboxen/PDMS涂层；每次进样前萃取头250℃预先老化15min，将老化好的纤维头插入样品瓶中顶空部分120℃萃取5min，然后将纤维头插入气相色谱-质谱联用仪进样口，250℃解吸15min，进行气相色谱-质谱联用检测；
C、气相色谱条件：气相色谱-质谱联用仪，载气为高纯度氦气，进样口温度270℃，色谱柱流量2mL/min；分流比10:1；
D、质谱条件：电子轰击(EI，electron impact)离子源，离子源温度230℃，四级杆温度150℃，质量扫描范围m/z 29～550，溶剂延迟0.5min；
E、挥发性成分的分析：定性分析各组分经NIST.11Library标准谱库进行检索分析，确认挥发性成分；定量分析通过采用Aglient数据分析软件，以各组分峰面积占总峰面积的百分比来表示各种挥发性成分的相对含量。
进一步的，所述的步骤A中越冬麦苗长到20-25cm时进行取样。
进一步的，所述的步骤C中采用Agilent 7890B-5977B气相色谱-质谱联用仪，色谱柱型号为Agilent HP-5(60m×0.25μm×0.25mm)。
进一步的，所述的步骤C中升温程序：初始40℃，保持5min，然后以15℃/min升到280℃，保持5min，再以15℃/min升到305℃，保持5min。
本发明方法对两种长三角地区主栽大麦品种“花30”和“苏啤3号”的大麦幼苗进行挥发性成分检测，从两种大麦苗中分别鉴定出36种和52种挥发性成分。
本发明优点在于：
1、本发明基于顶空固相微萃取和气相色谱－质谱联用法测定大麦幼苗中挥发性成分，分析方法快速、简单、准确度高，弥补了以往通过水蒸气蒸馏法、溶剂萃取法等萃取挥发成分之后再进行分析的萃取不完全、溶剂残留、耗时间耗力等不足之处，能更真实的反应大麦幼苗中挥发性成分的组成，也具有环境友好的优点。同时，本分析方法对样品需求量小，可实现大量样本的批量快速分析，可为大麦幼苗的品质筛选提供可靠依据。
2、本发明通过对固相微萃取条件和色谱分析条件进行限定，萃取头老化时间15min，萃取5min既保证了萃取充分，又避免了萃取时间过长导致微量化合物被覆盖和实验时间的延长。通过对气象色谱色谱柱型号、载气流速和升温程序的限定使待测样品中多种挥发性成分在较短的时间内完全分离，从而能够准确地同时测定出待测样品中多种挥发性成分的相对含量，测试结果准确性好、灵敏度高、结果稳定，可用于大麦幼苗中挥发性成分的检测，从而明确了大麦幼苗中的挥发性成分，为大麦幼苗的种植加工和开发应用提供理论依据。
附图说明
图1是本发明实施例提供的“花30”大麦幼苗中挥发性成分的HS-SPME-GC-MS总离子流图。
图2是本发明实施例提供的“苏啤3号”大麦幼苗中挥发性成分的HS-SPME-GC-MS总离子流图。
具体实施方式
下面结合实施例对本发明提供的具体实施方式作详细说明。
实施例：“花30”和“苏啤3号”大麦幼苗中挥发性成分的检测和分析
1测试材料
测试材料为“花30”和“苏啤3号”两个品种的大麦幼苗，由上海市农业科学院生物技术研究所植物细胞工程研究室提供。2018年11月播种于上海市农业科学院实验田，条播种植，正常水肥管理，越冬麦苗长到20-25cm(6-7叶期)进行取样。
2主要仪器与设备
仪器型号：Agilent 7890B-5977B气相色谱-质谱联用仪；20mL钳口顶空样品瓶美国Agilent公司；萃取头型号：50/30μm DVB/Carboxen/PDMS涂层，美国Supelco公司。
3试验条件
3.1样品处理：新鲜的麦苗测试，直接采收的麦苗，蒸馏水洗净，吸干水分，在室温条件下5 000r/min匀浆备用。各取5g样品于顶空瓶中，封口，待测。将老化好的纤维头插入样品瓶中顶空部分120℃萃取5min，然后将纤维头插入气相色谱-质谱联用仪进样口，250℃解吸15min，进行GC-MS检测。
3.2萃取条件：萃取头型号，50/30μm DVB/Carboxen/PDMS涂层。每次进样前萃取头250℃预先老化15min，将老化好的纤维头插入样品瓶中顶空部分120℃萃取5min，然后将纤维头插入气相色谱-质谱联用仪进样口，250℃解吸15min，进行GC-MS检测。
3.3色谱条件：色谱柱型号为HP-5(60m×0.25μm×0.25mm)；载气99.999％高纯度氦气；进样口温度270℃；升温程序：初始40℃，保持5min，然后以15℃/min升到280℃，保持5min，再以15℃/min升到305℃，保持5min；色谱柱流量2mL/min；分流比10：1。
3.4质谱条件：电子轰击(EI，electron impact)离子源，离子源温度230℃，四级杆温度150℃，质量扫描范围m/z 29～550，溶剂延迟0.5min。
3.5挥发性成分的分析
定性分析各组分经NIST.11Library标准谱库进行检索分析，确认挥发性成分。定量分析通过采用Aglient数据分析软件，以各组分峰面积占总峰面积的百分比来表示各种挥发性成分的相对含量。
4检测结果
“花30”和“苏啤3号”大麦幼苗中挥发性成分的总离子流色谱图件图1、图2，横坐标为保留时间，纵坐标为总离子流的强度。挥发性成分的种类和相对百分含量详见表1、表2。
表1“花30”大麦幼苗中的挥发性成分及相对含量
根据总离子流色谱图(图1)，经NIST.11Library谱图库联机搜索，然后经过挑选所得到的挥发性成分名称、保留时间和相对含量如表1所示。对结果进行分析可知“花30”麦苗中鉴定出36种成分。包括15个醛类化合物(67.375％)、6个酮类化合物(14.221％)、4个醇类化合物(4.638％)、4个杂环化合物(呋喃、萘)(4.204％)、3个烃类化合物(1.018％)、2个酚类化合物(2.981％)、2个酸类化合物(1.32％)和1个酯类化合物(0.428％)。在鉴定出的化合物中，醛类成分相对含量最高，其中十五醛(36.651％)，具有清香味；2-己烯醛(5.197％)，又称青叶醛，具有新鲜的绿叶清香；苯乙醛(3.04％)，具有浓郁的玉簪花香气；糠醛(1.541％)具有甜味、烤面包味，焦糖味；异香兰素(1.122％)，也称异香兰醛，具有橄榄样香气和浓郁的奶香；十八烷醛(1.12％)又名椰子醛，呈强烈的椰子香气。酮类化合物相对含量次之，为14.221％，其中β-紫罗兰酮(11.835％)具有甜花香味。呋喃类化合物中的2-乙基呋喃(2.78％)含量较高，呈强烈焦香香气，低浓度时呈浓厚的甜香香气和咖啡似芳香风味。酚类化合物4-乙烯基-2-甲氧基苯酚(1.638％)，具有发酵香、炒花生香。醇类、烃类等其它类型化合物含量较少，对麦苗的气味贡献较小。
表2“苏啤3号”大麦幼苗中的挥发性成分及相对含量
根据总离子流色谱图2，经谱图库搜索，所得的挥发性物质名称、保留时间和相对含量如表2所示。由表2可得，“苏啤3号”麦苗中鉴定出52种成分，包括21个醛类化合物(37.757％)、9个烃类化合物(6.38％)、7个醇类化合物(12.442％)、4个酮类化合物(10.847％)、4个杂环化合物(呋喃、萘)(9.885％)、2个酚类化合物(15.391％)、2个含氮化合物(胺、吲哚)(1.441％)、1个酯类化合物(0.188％)、1个酸类化合物(0.398％)。在鉴定出的化合物中除了与“花30”相同的成分外，苯甲醛(4.061％)具有强烈的香甜气味；壬醛(1.881％)具有强烈的油脂气味和甜橙气息；正己醛(1.307％)呈生的油脂和青草气及苹果香味；β-环柠檬醛(1.034％)具有凉香、果香和清香。酮类化合物相对含量为10.847％，对气味贡献较大的也为具有甜花香味的β-紫罗兰酮。
由表1与表2的分析结果可知，新鲜麦苗中挥发性成分主要为醛类和酮类，醛类化合物具有花香气味，可与许多其他物质产生很强的风味协同作用，酮类成分普遍有花香和果香风味，因此这两种成分与麦苗特殊清香有密切关系，是麦苗中的特征性挥发成分。
以上已对本发明创造的较佳实施例进行了具体说明，但本发明创造并不限于所述实施例，熟悉本领域的技术人员在不违背本发明创造精神的前提下还可做出种种的等同的变型或替换，这些等同的变型或替换均包含在本申请权利要求所限定的范围内。
Claims (4)
1.一种大麦幼苗挥发性成分的检测方法，其特征在于，包括以下步骤：
A、样品处理：越冬麦苗长到6-7叶期进行取样，采收的麦苗蒸馏水洗净，吸干水分，在室温条件下5 000r/min匀浆备用；取5g样品于顶空瓶中，封口，待测；
B、萃取条件：萃取头型号，50/30μm DVB/Carboxen/PDMS涂层；每次进样前萃取头250℃预先老化15min，将老化好的纤维头插入样品瓶中顶空部分120℃萃取5min，然后将纤维头插入气相色谱-质谱联用仪进样口，250℃解吸15min，进行气相色谱－质谱联用检测；
C、气相色谱条件：气相色谱-质谱联用仪，载气为高纯度氦气，进样口温度270℃，色谱柱流量2mL/min；分流比10:1；
D、质谱条件：电子轰击离子源，离子源温度230℃，四级杆温度150℃，质量扫描范围m/z29～550，溶剂延迟0.5min；
E、挥发性成分的分析：定性分析各组分经NIST.11Library标准谱库进行检索分析，确认挥发性成分；定量分析通过采用Aglient数据分析软件，以各组分峰面积占总峰面积的百分比来表示各种挥发性成分的相对含量。
2.根据权利要求1所述的大麦幼苗挥发性成分的检测方法，其特征在于，所述的步骤A中越冬麦苗长到20-25cm时进行取样。
3.根据权利要求1所述的大麦幼苗挥发性成分的检测方法，其特征在于，所述的步骤C中采用Agilent 7890B-5977B气相色谱-质谱联用仪，色谱柱型号为Agilent HP-5。
4.根据权利要求1所述的大麦幼苗挥发性成分的检测方法，其特征在于，所述的步骤C中升温程序：初始40℃，保持5min，然后以15℃/min升到280℃，保持5min，再以15℃/min升到305℃，保持5min。
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