CN103645258B - 一种木香乙酸乙酯提取物的检测方法 - Google Patents
一种木香乙酸乙酯提取物的检测方法 Download PDFInfo
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Abstract
本发明涉及木香乙酸乙酯提取物的检测方法，具体涉及一种联用UPLC和Q-TOF-MS来检测木香乙酸乙酯提取物具体成分的方法，色谱条件为：二元梯度洗脱，A相为水溶液，B相为乙腈，流速0.3mL/min；进样量4μL；质谱条件为：采用电喷雾电离源，TOF离子飞行方式采用正离子模式检测，该检测方法为木香的乙酸乙酯提取物质量评价提供了一种手段，有利于进一步制定木香的乙酸乙酯提取物的质量监控。
Description
[技术领域]
本发明涉及木香乙酸乙酯提取物的检测方法，具体涉及一种联用UPLC和Q-TOF-MS来检测木香乙酸乙酯提取物具体成分的方法。
[背景技术]
木香，中药名。为菊科植物木香Aucklandia lappa Decne.的干燥根。始载于《神农本草经》列为上品,味辛苦,性温,具有行气止痛,健脾消食的功效,临床上用于胸脘胀痛、泻痢后重,食积不消,不思饮食等症,煨制后涩肠止泻,用于泄泻腹痛,为治疗腹痛、泻痢的常用药。《名医别录》称之为蜜香、青木香。李时珍谓:“昔人谓之青木香,后人因呼马兜铃根为青木香,乃呼此为南木香,广木香以别之。”在配方过程中,医生处方中常见有云木香,川木香,土木香,青木香,红木香及越西木香等带有“木香”之名出现,容易不致混淆。
木香的鉴别方法有性状鉴别、显微鉴别，具体为：
性状鉴别为：略呈圆柱形,枯骨形为纵剖片,长约5～15cm,直径0·5～6cm,表面黄褐色,栓皮多除去,有显著纵沟及侧根痕,有时可见不规则菱形网纹。质坚实,体重,不易折段。断面略平坦,黄白色至棕黄色,有一棕色环及放射性纹理,并可见散在的褐色油点。气强烈芳香,味苦。
显微鉴别为：1.横切面：木栓层为多列木栓细胞；韧皮部宽广,射线明显，成环状；木质部木质部导管单行径向排列，木纤维存于近形成层处及中心的导管旁,初生木质部多为四圆形；油室散在于薄壁细胞中,呈圆形或椭圆形,常贮有黄色油滴；薄壁细胞含有菊糖。2.粉末：菊糖极多；木纤维多成束长菱形,直径16～24Lm,纹孔口横裂孔状,十字状或人字状；导管主为网纹导管,也有具缘纹导管,直径30～90Lm；油室可见油室碎片,内含黄色或棕色分泌物；
木栓细胞淡黄棕色。表面观类多角形,大小不一,垂周壁微波状弯曲。
而关于木香提取物及有效成分的检测也很少有报道，例如：
国内申请201210425189X公开了一种木香的乙酸乙酯提取物，其制备方法为：木香用石油醚浸泡18-36h，渗滤提取至3-8倍药材量，回收残渣，挥干残渣中的石油醚，用70%-90%乙醇提取，提取液浓缩得乙醇浓缩液，用乙酸乙酯萃取，倒出上层，即得乙酸乙酯提取物。但是没有提及该产品的检测或鉴别方法。
UPLC/Q-TOF-MS分析方法是超高效液相色谱-四极杆联合飞行时间串联质谱分析方法，通过高效液相的联用，可以方便得到每个样品的主要结构信息，并针对每个组分进行准确的定性分析。四级杆质谱是在交变电场的作用下没事某些符合要求的离子通过四级杆到达检测器，飞行时间质谱（TOF）是应用不同的m/z离子的飞行速度不同，离子飞行通过相同的路径到达检测器的时间不同而获得质量分离。四级杆串联飞行时间质谱不仅用于一级质谱的分析而且可以实现二级质谱分析，一级质谱可得出化合物的分子量信息，二级质谱则可以得到化合物的碎片离子等结构信息。
目前，UPLC/Q-TOF-MS可以广泛运用中药化学成分的快速鉴定定性分析，它可以使样品的分离和定性及定量成为一个连续的过程，费时费力而且对环境不好，UPLC/Q-TOF-MS的快速分析鉴别，能够在短时有效成分分离的基础上，获得大量的化合物结构信息，在中药化学成分分析中发挥了重要的作用。
[发明内容]
为了弥补现有技术的不足，本发明提供了能够检测类似国内申请201210425189X的木香乙酸乙酯提取物的方法，并通过联用UPLC和Q-TOF-MS来实现。
为实现上述目的，设计一种木香乙酸乙酯提取物的检测方法，联用UPLC和Q-TOF-MS进行分析检测，所述的方法由以下步骤组成：
a.所述的UPLC分析的条件为：采用Waters ACQUITY UPLCTM BEH C18Column(50mm×2.1mm.id.,1.7μm)柱进行二元梯度洗脱，A相为水溶液，B相为乙腈，流速0.3mL/min；进样量3～4μL；
b.所述的Q-TOF-MS分析的条件为：采用电喷雾电离源、TOF离子飞行和正离子模式检测，四级杆质量扫描范围为50～1200m/z，一次扫描时间为0.1s，离子源温度120℃，去溶剂温度300℃，锥孔气体流速为50L/h，脱溶剂氮气流速800L/h，正离子电离模式，毛细管电离电压3kV，锥孔电压40V，碰撞气体压力为2.5×10-3Mbar，电子倍增器电压650V。
所述的梯度洗脱的具体优化步骤如下：
所述的进样量优选为4μL。
本发明提供的木香的乙酸乙酯提取物的检测方法具有以下优点：
1、本发明应用超高效液相色谱-质谱联机分析技术及结果构建木香的乙酸乙酯提取物的指纹图谱的方法。该方法包括木香的乙酸乙酯提取物的UPLC-MS分析条件。色谱峰的特征、色谱组分的质谱提供的化合物结果信息等。本发明公开的指纹图谱及其技术可用于木香的乙酸乙酯提取物的品种鉴别及木香提取物的质量监控。
2、经UPLC/Q-TOF-MS分析，能够较全面的反映出木香的乙酸乙酯提取物主要成分为倍半萜类，去氢木香内酯，木香烃内酯，木香醇,正戊基呋喃，姜黄烯，7,8-二氢紫罗兰酮。
[附图说明]
图1：木香的乙酸乙酯提取物UPLC分析色谱图；
图2：木香的乙酸乙酯提取物UPLC-ESI-MS(+)分析总离子流色谱图。
[具体实施方式]
为了使本发明的目的、技术方案及优点更加清楚明白，结合附图对本发明进行进一步详细说明。本申请中的生产设备都是本领域的常用设备，应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
检测试剂
甲醇为色谱纯，美国Fisher公司;
超纯水，实验室ELGA PURELAB Classic-UVF纯水机制备，该纯水机购自英国；
其他试剂均为市售国产分析纯。
检测样品
制备在国内申请201210425189X中实施例1制备的木香的乙酸乙酯提取物，样品的具体制备方法为：药材样品粉碎成粗粉，取粗粉500克，先用石油醚浸泡1天后渗滤提取至提取液颜色浅（或5倍药材量），回收石油醚，得石油醚提取物；残渣挥去石油醚，用80%乙醇湿润后，再用3倍量80%乙醇回流提取两次，合并提取液，减压回收乙醇至无醇味，用等体积乙酸乙酯萃取2次，合并乙酸乙酯萃取液，回收乙酸乙酯至干，得乙酸乙酯萃取物；母液浓缩至干，得乙醇提取物；残渣挥干乙醇，用3倍量水煮提2次，合并水提取液，浓缩至干，得水提取液。
实验条件
色谱条件为：色谱柱：Waters ACQUITY UPLCTM BEH C18Column(50mm×2.1mm.i d.,1.7μm)柱；柱温：35℃；流动相：二元梯度洗脱，A相为水溶液，B相为乙腈；流速0.3mL/min；每次进样量4μL，其梯度洗脱的的条件为：
表1：梯度洗脱
Q-TOF MS条件，质谱采用电喷雾电离源（ESI），TOF离子飞行方式采用Ⅴ模式；四级杆质量扫描m/z范围50-1200，一次扫描时间为0.1s，离子源温度120℃，去溶剂温度300℃，锥孔气体流速为50L/h，脱溶剂氮气流速800L/h，正离子电离模式，毛细管电离电压3kV，锥孔电压40V，碰撞气体压力为2.5×10-3Mbar,电子倍增器电压650V。
数据处理，UPLC-MS的原始数据文件通过Waters Micromass Mass V4.1数据处理系统获得，对于每个离子的鉴定通过正离子和负离子模式下的二级质谱进一步确认。
实验结果：见图1、图2和表2
图1为木香的乙酸乙酯提取物的UPLC图，图2为木香的乙酸乙酯提取物的UPLC-ESI-MS(+)分析总离子流色谱图，对图2中的总离子流色谱峰组分进行指纹信息分析，得到表2内容：
表2：木香提取物的总离子流色谱峰组分指纹信息
表2结果显从木香的乙酸乙酯提取物中分析鉴定出7个化学物，主要成分为倍半萜类化合物，分别是去氢木香内酯，木香醇，正戊基呋喃，木香烃内酯，姜黄烯，7,8-二氢紫罗兰酮。
通过现有技术可知：本发明提供的UPLC/Q-TOF-MS可以检测木香的乙酸乙酯提取物中倍半萜类化合物，可以作为一种有效地鉴定木香药材的方法。
虽然，上文中已经用一般性说明、具体实施方式及试验，对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。
Claims (2)
1.一种木香乙酸乙酯提取物的检测方法，联用UPLC和Q-TOF-MS进行分析检测，其特征在于所述的方法由以下步骤组成：
a.所述的UPLC分析的条件为：采用Waters ACQUITY UPLCTM BEH C18柱，50mm×2.1mm.i d.,1.7μm进行二元梯度洗脱，A相为水溶液，B相为乙腈，流速0.3mL/min；进样量3～4μL；
b.所述的Q-TOF-MS分析的条件为：采用电喷雾电离源、TOF离子飞行和正离子模式检测，四级杆质量扫描范围为50～1200m/z，一次扫描时间为0.1s，离子源温度120℃，去溶剂温度300℃，锥孔气体流速为50L/h，脱溶剂氮气流速800L/h，正离子电离模式，毛细管电离电压3kV，锥孔电压40V，碰撞气体压力为2.5×10-3Mbar，电子倍增器电压650V；
c.所述的梯度洗脱的具体步骤如下：
。
2.如权利要求1所述的木香乙酸乙酯提取物的检测方法，其特征在于所述的进样量为4μL。
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