两种凤丹鲜花挥发性成分的HS/SPME/GC/MS分析

利用顶空固相微萃取/气相色谱/质谱(HS/SPME/GC/MS)联用技术对凤丹白和凤丹粉两种鲜花的挥发性成分进行研究,比较分析两种凤丹鲜花挥发性成分.两种凤丹鲜花中共检测出50种挥发性成分,其共有的挥发性成分有27种.在凤丹白鲜花中检测出41种挥发性成分,占挥发性总成分的89.00％,主要为碳氢类、醛类、醚类、醇类、酚类和酯类化合物,分别占挥发性总成分的55.78％、21.15％、9.22％、2.32％、0.27％和0.26％;在凤丹粉鲜花中检测出36种挥发性成分,占挥发性总成分的89.00％,主要为碳氢类、醚类、醇类、醛类、酯类和酚类化合物,分别占挥发性总成分的78.76％、4.07％、2.72％、2.70％、0.42％和0.33％.两种凤丹鲜花挥发性成分及含量差异比较显著,差异性成分主要表现为:凤丹白含有(R)-3,7-二甲基-6-辛烯醛、壬醛、正己醛、2,2,4,6,6-五甲基-庚烷等,而凤丹粉含有6,9-十七烷二烯.     

金银忍冬果实中挥发性成分的GC-MS分析

研究宁夏生长的金银忍冬果实中挥发性物质的化学成分.用乙醚作溶剂,采用索氏提取法从宁夏生长的金银忍冬果实中提取挥发性物质,并通过GC-MS联用技术对挥发性成分进行了分析鉴定,用色谱峰面积归一化法计算了各成分的相对含量.从宁夏生长的金银忍冬果实中提取的挥发性物质中鉴定了32种化合物,其中含量最大的是甲基己基过氧化氢(1.3...     

浙产竹叶椒不同部位挥发性成分的GC-MS分析比较

分析浙产竹叶椒不同部位的挥发性化学成分.用水蒸气蒸馏法提取挥发性成分,采用气相色谱-质谱联用法(GC-MS)测试,并用面积归一化法计算出各组分的相对百分含量.通过计算机自动检索,从浙产竹叶椒叶、茎皮和果实中分离鉴定出的组分数分别为60、16和12.浙产竹叶椒叶、茎皮和果实3个部位的挥发性成分及含量存在很大的区别,可为进...     

普洱茶挥发性成分的GC-MS分析

采用同时蒸馏萃取法(SDE)提取普洱茶的挥发性成分,经气质联用分析鉴定,应用色谱峰面积归一化测定各成分的相对含量。经过对该茶样的分析,共鉴定出44种挥发性成分,占挥发性成分总量的92.46%,其中含量较高的化合物有醇类、酯类、酸类和苯衍生物,它们分别占总量的15.47%、12.43%、8.74%、32.36%。     

蓝花喜盐鸢尾和喜盐鸢尾的化学成分比较分析

采用气相色谱-质谱联用法结合计算机谱图检索,对蓝花喜盐鸢尾根的脂溶性成分和喜盐鸢尾根的挥发性进行分析比较.结果表明:蓝花喜盐鸢尾根和喜盐鸢尾根共鉴定出41种成分.二者共有的成分为(E,E)-9,12-十八二烯酸甲酯、(Z)-9-十八烯酸甲酯.蓝花喜盐鸢尾与喜盐鸢尾成分相比较组成和相对含量存在着较大差异.研究结果有利于鸢...     

不同生长期当归1H NMR指纹图谱的研究

利用¹H NMR法测定27个不同生长期的当归提取物,对当归的主要活性成分阿魏酸、藁本内酯、当归多糖进行了初步归属,用特征峰相对峰面积表示3种活性成分的相对含量,并对它们在生长过程中的含量变化进行分析. 数据分析显示,当归中阿魏酸、藁本内酯、当归多糖的含量在第1年变化较为平稳,第2年和第3年变化相对较为活跃,而在当归的生长周期内,当归多糖的含量变化明显大于其他两种活性成分,为参与代谢活动的主要活性成分. 结果证实,通过对照¹H NMR指纹图谱, 将相对含量法与主成分分析法相结合,能对不同生长期的当归药材中的活性成分进行宏观评价和分析,可作为植物药材代谢组学的研究方法.     

5种产地九节菖蒲脂溶性成分GC-MS比较分析

分析鉴定和比较5种产地九节菖蒲中的脂溶性成分.采用索氏提取法提取脂溶性成分,甲酯化后采用气相色谱-质谱(GC-MS)联用技术分离并鉴定其组分,并用面积归一化法计算出各组分的相对百分含量.宁夏、山西、河南、四川和陕西九节菖蒲中分别鉴定出18、22、20、20种和20种脂溶性成分.5种产地九节菖蒲中的共有成分为8个,共有主成分为棕榈酸和亚油酸.不同产地九节菖蒲中脂溶性成分组成及相对含量差异较大,可为九节菖蒲的鉴别和临床应用提供参考.     

5种鹿茸营养成分的主成分分析

对梅花鹿茸、马鹿茸、花马杂交鹿茸、麋鹿茸及驯鹿茸等五种鹿茸的常规成分、无机元素和氨基酸含量进行了测定.采用原子吸收光谱法测定了15种无机元素的含量;使用氨基酸分析仪结合分光光度法测定了五种鹿茸不同部位的17种氨基酸的含量.采用主成分分析法对鹿茸的营养成分进行分析,探讨了不同品种鹿茸的差异及特征成分.结果表明,粗蛋白、Ca、P、Na、Fe、Ba、Sr、谷氨酸及甘氨酸是鹿茸的特征成分,与鹿茸品质特征密切相关.根据无机元素含量的主成分分析得分图,可将梅花鹿茸、麋鹿茸与其他3种鹿茸区分,而常规成分和氨基酸的主成分得分图不能明显表征五种鹿茸的差异.主成分分析揭示了不同鹿茸在营养成分上的相似性和差异性.本研究为鹿茸的进一步开发利用提供重要依据.     

茶叶及其组份的红外光谱研究

采用光学方法针对四种茶叶及其四种主要组份在800～3800 cm-1中红外"指纹"特征区域的光谱进行系统研究,采集了不同产地的碧螺春和铁观音以及决定茶叶品质的主要成份中咖啡因、谷氨酸和表儿茶素和花青素类物质的中红外光谱.通过建立模型对各特征光谱进行主成份拟合分析了茶叶品种、产地差异与各主要成份含量的关系.结果表明,不同茶叶之间的差异可表现在其主成份相对含量上:对于不同种类茶叶的碧螺春和铁观音,差异主要表现在茶叶有效成份的含量不同,前者中的各组份含量相对较低;对于不同产地的同种茶叶,差异主要表现在咖啡因和表儿茶素的相对含量不同,其中原产地茶叶中含量相对较高.此研究为利用光学方法对茶叶的种类和品质实现快速检测提供重要参考.     

近红外漫反射光谱法快速测定畜禽粪便堆肥多组分含量

以我国22个省、市120个不同种类的畜禽粪便堆肥样品为研究对象,利用傅里叶变换近红外漫反射光谱技术和偏最小二乘回归法建立了我国畜禽粪便堆肥中水分、挥发性固体、总有机碳、总氮含量、碳氮比、酸碱度和电导率的近红外定量分析校正模型。各参数校正模型的决定系数R2分别为0.981 6,0.901 5,0.961 0,0.987 4,0.741 0,0.788 0和0.870 4;验证集决定系数R2_v分别为0.983 2,0.938 1,0.912 8,0.973 5,0.830 8,0.615 8和0.895 3。研究发现,除酸碱度近红外模型相对分析误差RPD(SD/SEP)值小于2.0外,水分、挥发性固体、总有机碳、总氮含量和电导率近红外模型的相对分析误差RPD值均大于3.0;碳氮比近红外模型相对分析误差RPD值介于2.0到2.5之间。结果表明,近红外漫反射光谱法可以快速测定畜禽粪便堆肥中水分、挥发性固体、总有机碳、总氮含量和电导率,对碳氮比的测定精度有待于进一步提高,对酸碱度的预测效果不理想。     

蛇百子中挥发油成分的GC-MS分析

对蛇百子全草中挥发油部分进行分析,研究其化学成分。采用水蒸气蒸馏法提取获得总挥发油（Ⅰ）,乙醚萃取得到挥发油（Ⅱ）,再用乙酸乙酯进一步提取得到挥发油（Ⅲ）,通过GC-MS技术对其进行分析。共分离鉴定出化学成分48种,其中挥发油（Ⅰ）鉴定出36种化合物、挥发油（Ⅱ）鉴定出30种化合物、挥发油（Ⅲ）鉴定出10种化合物。挥发油的主要成分为反式石竹烯、1,8-桉树脑、侧柏烯、α-香柑油烯、β-榄香烯、桉树脑、γ-古芸烯等。     

紫外光谱法分析煤直接液化油族组成

煤液化油组成的测定方法以色谱法为主,但由于样品沸程长,组分性质不均一,色谱法无法实现简便快速地对液化油族组分进行定性/定量。为建立一种快速准确定量煤液化油中的酚类化合物、芳烃、脂肪烃的分析方法,本文选取具有代表性组成的煤液化油180～200 ℃馏分为研究对象,筛选了环己烷、乙醇、氢氧化钠-乙醇(50 Wt%,简称碱醇溶剂)三种分离溶剂。通过对煤液化油样品在200～400 nm波长间的特征吸收峰分析,发现碱醇溶剂可使芳烃化合物对酚类化合物的干扰减少到最小,可以有效避免吸收峰重叠问题。在此基础上,进一步对比分析了苯酚,间甲酚,邻甲酚,对甲酚等标准化合物与液化油酚类混合物在碱醇溶液中紫外吸收的标准曲线,以定量样品组成。选择间甲酚为标准化合物,根据其在290 nm处的标准曲线,得到煤液化油中酚类化合物的总量为32.14%,测定结果与宏量样品分离、称重、物料平衡后结果基本一致。在得到酚类化合物含量之后,以四氢萘为标准物,获得液化油中芳烃的总量为44.91%,脂肪烃的含量为22.95%。为确定方法的准确性,油样分别加入不同量的间甲酚和四氢萘标准物,酚的加标回收率为104.3～110.75%,芳香烃的加标回收率在84.3～91.75%。综上表明：利用紫外光谱法,以碱醇溶剂排除芳烃对酚吸收的影响,能够快速测定煤液化油中酚类和芳香烃的含量,脂肪烃的含量可差减得到。     

顶空固相微萃取-气相色谱-质谱联用分析马蹄香中的挥发油成分

利用顶空固相微萃取-气相色谱-质谱联用技术分析马蹄香挥发油的化学成分,为马蹄香的挥发油成分分析提供新方法。以顶空固相微萃取法提取挥发油,气相色谱-质谱联用技术对挥发油成分进行分离鉴定,并采用面积归一化法确定各成分的相对质量分数。结果样品在90℃下平衡30min,顶空吸附15min的条件下,采用100μm PDMS纤维头能有效地吸附马蹄香挥发油成分。气相色谱-质谱联用技术共鉴定出57个成分,其中相对质量分数较高的有西车烯(15.93%)、1,2,3,5,6,7,8,8a-八氢-1,4-二甲基-7-(1-甲基乙烯基)甘菊蓝(13.55%)、α-广藿香烯(9.50%)等。马蹄香挥发油具有丰富的化学成分,顶空固相微萃取-气相色谱-质谱联用能全面快速地获得其组成信息,可应用于马蹄香挥发油成分的研究。     

以香草素为内标之气相层析光谱法定量牛樟木精油指标成分松油醇的快速分析方法

牛樟精油具有独特浓郁的香气,其中以α-松油醇(α-terpineol)为牛樟精油主要成分。由于樟树精油制品可依种类、变种、亚种等不同而有不同成分,以松油醇最具独特性,可作为牛樟木精油品质重要指标成分,应用以区别牛樟树与冇樟以及香樟等木材精油的方法,因此建立市售牛樟木精油指标成分α-松油醇含量的简便快速又准确的检验方法便有其必要性。该研究拟以市售精油液体样品,不经任何前处理,加入适当之内标准溶液溶解后,直接注入气相层析光谱仪中,配合适当的分离管柱及气相层析条件,以期建立简便快速又准确的牛樟木精油指标成分α-松油醇之定量方法。毛细管柱气相层析具有高解析度及高灵敏度等优点,仍为现代最重要分析技术之一,因此研究建立了以香草素为内标准定量牛樟木精油指标成分α-松油醇(α-terpineol)之气相色谱层析法的快速分析方法。牛樟木精油液体样品,加入适当量之香草素内标准溶液混合溶解后,即可直接注入配有广口径之毛细管柱(megabore column)气相色谱仪中分析,相当简便,每分析一个样品仅需约30 min。结果显示松油醇之最低定量浓度（limit of quantitation, LOQ）为1 μg·mL-1左右。在添加回收试验中添加松油醇1.0及10.0 mg 于市售冇樟精油及牛樟精油中,其回收率在98%~103%,变异系数均在10.8%以下,显示该方法的精密度相当高。以该研究建立的方法分析15件市售牛樟精油中松油醇含量,结果显示,市售牛樟木精油的松油醇含量最高约51.6%及最低为21.3%左右,此结果显示以定量松油醇作为市售牛樟精油品质指标是一快速、准确且可行的方法。     

High power ultrasound effects on lipid oxidation of refined sunflower oil

The effects of high power ultrasound treatment (20 kHz) on some components of refined sunflower oil were studied in order to verify if and to what extent modifications in the lipidic fraction can occur. Traditional parameters including free acidity, total polar compounds, peroxide value, and conjugated dienes concentration were determined in refined sunflower oil samples before, immediately after the ultrasonic treatment and during storage. Differences between treated and untreated samples were detected only for peroxide values (PV). The PV increased from 5.38 meq. O2/kg oil for untreated oil to 6.33 meq. O2/kg oil for sunflower oil sonicated (20 kHz; 150 W; 2 min). The fatty acid composition was obtained by high resolution gas chromatography. No significant changes were observed regarding the decrease in fatty acid composition before and immediately after the treatment. Regarding the volatile fraction, some off-flavour compounds for example hexanal and limonene resulting from the ultrasonic degradation of sunflower oil were identified by gas chromatography coupled to mass spectrometry (GC-MS).     

近红外光谱法快速测定新疆薰衣草精油主要组分

为建立快速测定新疆薰衣草精油中芳樟醇(linalool)、乙酸芳樟酯(linalyl acetate)含量的定量分析模型,采用近红外吸收光谱法(NIR)测定了165个精油样品,通过对近红外光谱吸收峰分析,在7 100～4 500 cm-1波数范围内化学信息量比较丰富且噪音低,可选择此波数段为分析区间。剔除8个异常样本后,通过聚类方法划分为105个校正集样本和52个验证集样本,结合气相色谱质谱(GC-MS)法测定的薰衣草精油linalool和linalyl acetate的含量,建立原始数据矩阵。对比不同的预处理方法对原始近红外光谱的过滤作用,其中正交信号变换(OSC)方法效果明显,对两种化合物的预测均方根误差(RMSEP) 分别为0.226和0.558,再用向前间隔偏最小二乘法(FiPLS)剔除与待测成分无关或呈非线性关系的波长点,最终得到8个间隔区间共160个波长点的数据子集。使用OSC-FiPLS优化处理的数据子集结合偏最小二乘法(PLS)建立新疆薰衣草精油中linalool和linalyl acetate的快速定量分析模型,在模型中二成分的隐变量数都为8。交互验证均方根误差(RMSECV)分别为0.170和0.416;预测均方根误差(RMSEP)分别为0.188和0.364。结果表明,经OSC和FiPLS预处理建立的PLS-NIR定量分析模型稳健性好,测定精度高,能快速测定薰衣草精油中linalool和linalyl acetate含量,并且具有良好的预测能力。可为新疆薰衣草精油主要成分的快速定量分析提供一种新的有效方法。     

Main Components of Xinjiang Lavender Essential Oil Determined by Partial Least Squares and Near Infrared SpectroscopySCIEI北大核心CSCD

This work was undertaken to establish a quantitative analysis model which can rapid determinate the content of linalool, linalyl acetate of Xinjiang lavender essential oil. Totally 165 lavender essential oil samples were measured by using near infrared absorption spectrum(NIR), after analyzing the near infrared spectral absorption peaks of all samples, lavender essential oil have abundant chemical information and the interference of random noise may be relatively low on the spectral intervals of 7100-4 500 cm(-1). Thus, the PLS models was constructed by using this interval for further analysis. 8 abnormal samples were eliminated. Through the clustering method, 157 lavender essential oil samples were divided into 105 calibration set samples and 52 validation set samples. Gas chromatography mass spectrometry (GC-MS) was used as a tool to determine the content of linalool and linalyl acetate in lavender essential oil. Then the matrix was established with the GC-MS raw data of two compounds in combination with the original NIR data. In order to optimize the model, different pretreatment methods were used to preprocess the raw NIR spectral to contrast the spectral filtering effect, after analysizing the quantitative model results of linalool and linalyl acetate, the root mean square error prediction(RMSEP) of orthogonal signal transformation (OSC) was 0.226, 0.558, spectrally, it was the optimum pretreatment method. In addition, forward interval partial least squares (FiPLS) method was used to exclude the wavelength points which has nothing to do with determination composition or present nonlinear correlation, finally 8 spectral intervals totally 160 wavelength points were obtained as the dataset. Combining the data sets which have optimized by OSC-FiPLS with partial least squares(PLS) to establish a rapid quantitative analysis model for determining the content of linalool and linalyl acetate in Xinjiang lavender essential oil, numbers of hidden variables of two components were 8 in the model. The performance of the model was evaluated according to root mean square error of cross-validation (RMSECV) 9 root mean square error of prediction (RMSEP). In the model, RESECV of linalool and linalyl acetate were 0.170 and 0.416, respectively; RMSEP were 0.188 and 0.364. The results indicated that raw data was pretreated by OSC and FiPLS, the NIR-PLS quantitative analysis model with good robustness, high measurement precision; it could quickly determine the content of linalool and linalyl acetate in lavender essential oil. In addition, the model has a favorable prediction ability. The study also provide a new effective method which could rapid quantitative analysis the major components of Xinjiang lavender essential oil.     

Environmental monitoring based on NMR analysis of the composition of essential oil from Canadian spruce needles

We have used ¹H and ¹³C NMR spectroscopy to analyze the chemical composition of essential oil from needles of Canadian spruce (Picea glauca (Moench) Voss) grown in different regions of the Republic of Belarus. We consider the change in the composition of the oil depending on the area where the spruce was grown. We suggest using spruce needle essential oil as a biological indicator for environmental conditions in the area.     

SPME/GC/MS分析小一点红挥发性化学成分

利用固相微萃取/气相色谱/质谱(SPME/GC/MS)联用技术对小一点红挥发性成分进行研究。共鉴定出25种化学成分,占挥发性总成分的91.99%。小一点红主要挥发性化学成分是β-月桂烯(51.18%),3,7,11,15-四甲基-2-十六烯-1-醇(21.55%),β-水芹烯(8.42%),n-十六酸(2.48%)等。     

Comparison of distillation and ultrasound-assisted extraction methods for the isolation of sensitive aroma compounds from garlic (Allium sativum)

A comparative study of traditional simultaneous distillation extraction (SDE), microwave assisted hydrodistillation extraction (MWHD) and ultrasound-assisted extraction (USE) is presented, for the extraction of essential oils from fresh garlic (Allium sativum) cloves. Each method is evaluated in terms of qualitative and quantitative composition of the isolated essential oil. The highly reactive sulfur molecules of the garlic volatile fraction show variable response to the different isolation methods. The application of ultrasound for the extraction of the essential oil is considered to cause a lesser damage of thermal-sensitive molecules, thus, providing a better approach of the compounds primarily responsible for the characteristic odor and taste of freshly chopped garlic. All heat-involving isolation procedures have been shown to differentiate the volatile-fraction profile as analyzed by GC-MS. Especially when grouping the compounds into cyclic and acyclic, the percentage concentrations drop from 77.4% to 8.7% for the acyclic while that of the cyclic compounds increase from 4.7% to 70.8%. The observed fact may be attributed to the effect of the heat applied, which changes from harsh thermal treatment (SDE) to short time thermal (MWHD) and room-temperature isolation (USE). The use of USE proves to be crucial in order to provide reliable insight into garlic's chemistry.