HS-SPME-GC-MS法检测并鉴定胡椒叶和果实中的挥发性成分
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篇名: HS-SPME-GC-MS法检测并鉴定胡椒叶和果实中的挥发性成分
TITLE:
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 mL/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 eV,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。
ABSTRACT: 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 mL/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 eV, 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 for 67.13% 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.
期刊: 2017年第28卷第6期
作者: 张伟,张娟娟,尹震花,张勇,康文艺
AUTHORS: ZHANG Wei,ZHANG Juanjuan,YIN Zhenhua,ZHANG Yong,KANG Wenyi
关键字: 胡椒;挥发性成分;顶空固相微萃取;气质联用
KEYWORDS: Piper nigrum; Volatile constituents; HS-SPME; GC-MS
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