HS-SPME-GC-MS法检测并鉴定胡椒叶和果实中的挥发性成分  

Detection and Identification of Volatile Constituents from Leaves and Fruits of Piper nigrum by HSSPME-GC-MS

作　　者：张伟[1] 张娟娟[1] 尹震花[1] 张勇[1] 康文艺[1] 

机构地区：[1]黄河科技学院医学院,郑州450063

出　　处：《中国药房》2017年第6期820-822,共3页China Pharmacy

基　　金：河南省重点科技攻关项目(No.152102310171);郑州市科技发展计划项目(No.20150341)

摘　　要：目的:检测并鉴定胡椒叶和果实中挥发性成分的方法。方法:采用顶空固相微萃取-气相色谱-质谱联用法(HS-SPME-GC-MS)。色谱条件:色谱柱为HP-5 MS石英弹性毛细管柱,载气为高纯氦气(99.999%),流速为1.0 m L/min,进样口温度为250℃,色谱柱初始温度为50℃(程序升温),分流进样,分流比为10∶1。质谱条件:电离方式为电子轰击离子源,电离能量为80 e V,离子源温度为230℃,四极杆温度为150℃,传输线温度为280℃,电子倍增器电压为1 588 V,质量扫描范围为m/z 30~400。采用RTLPEST3.L和NIST08.L谱库进行谱图检索,以面积归一化法测定各挥发性成分的相对含量。结果:从胡椒叶中鉴定出28个挥发性成分,果实中鉴定出15个化合物,分别占总峰面积的67.13%、36.85%。其中,叶中主要挥发性成分为β-石竹烯(15.72%)、柠檬烯(9.39%)、3-蒈烯(9.32%)、β-蒎烯(6.80%)和α-萜品烯(4.98%)等,果实中主要挥发性成分为1,7,7-三甲基-2-乙烯基二环[2.2.1]庚-2-烯(10.45%)、匙桉醇(8.28%)和氧化石竹烯(4.81%)等;二者有5个共有成分。结论:该研究基本明确了胡椒叶和果实中主要挥发性成分,并且证实了二者存在明显差异。OBJECTIVE：To establish a method for the detection of volatile constituents from the leaves and fruits of Piper nigrum. METHODS：HS-SPME-GC-MS was used. The chromatographic conditions：column was HP-5 MS quartz elastic capillaries,carrier gas was high purity helium（99.999%）,flow rate was 1.0 m L/min,the inlet temperature was 250 ℃,initial temperature of column was 50 ℃（temperature programmed）,split injection with split ratio of 10 ∶ 1. MS conditions：ionization mode was electron impact ion source,ionization energy was 80 e V,ion source temperature was 230 ℃,quadrupole temperature was 150 ℃,transmission line temperature was 280 ℃,electron multiplier voltage was 1 588 V,mass scanning range was m/z 30-400. The spectra were retrieved using RTLPEST3. L and NIST08. L,and the relative contents of the volatile constituents were determined by area normalization method. RESULTS：There were 28 volatile constituents in the leaves and 15 in the fruits,respectively accounting for67.13% and 36.85%. The major volatile constituents of leaves were β-caryophyllene（15.72%）,limonene（9.39%）,3-carene（9.32%）,β-pinene（6.80%）,α-terpine（4.98%）,etc.,the main volatile constituents of fruits were 1,7,7-trimethyl-2-vinylbicyclo[2.2.1]hept-2-ene（10.45%）,espatulenol（8.28%）,caryophyllene oxide（4.81%）,etc. 5 constituents were owned in both. CONCLUSIONS：The study basically clears the main volatile constituents from the leaves and fruits of P. nigrum,and verifies existing obvious differences.

关 键 词：胡椒 挥发性成分 顶空固相微萃取 气质联用 

分 类 号：R284.1[医药卫生—中药学]