离子色谱法同时测定果汁中20种有机胺、生物胺和阳离子

建立了梯度淋洗-电导抑制-离子色谱法测定果汁中20种有机胺、生物胺和阳离子的方法,通过对流速、色谱柱温度、p H等因素的考察,探索出了适合20种组分测定的多级梯度淋洗条件。结果表明,当流速为0. 25 mL/min,pH在3. 5～4. 5,柱温在40℃时,20种组分在0. 05～2. 00 mg/L浓度范围内具有良好的线性关系(R 0. 99)。20种组分检出限(S/N=3)在0. 0006～0. 0503 mg/L之间;在0. 10,0. 20,1. 00 mg/L 3个添加浓度水平下,回收率为78. 4%～108. 9%,相对标准偏差(RSDs)在2. 1%～7. 3%之间。该方法适用于果汁中20种有机胺、生物胺和阳离子的分析测定。     

高效液相色谱法同时测定止咳宁嗽胶囊中3种活性成分

建立高效液相色谱法同时测定止咳宁嗽胶囊中3种活性成分绿原酸、金丝桃苷和橙皮苷的方法。色谱柱为非极性固定相TC–C_(18)柱(4.6 mm×250 mm,5μm);检测波长:0~10 min为327 nm,10~48 min为280 nm;流动相为乙腈–0.2%冰乙酸溶液,线性梯度洗脱,流量为1.0 mL/min;柱温为25℃;进样体积为10μL。3种活性成分的质量浓度与其色谱峰面积均呈现良好的线性关系,线性相关系数大于0.998,绿原酸、橙皮苷、金丝桃苷的检出限分别为1,2,10 ng/mL。测定结果的相对标准偏差小于4%(n=5),样品加标回收率为94.70%~100.40%。该法操作简便,结果可靠,适用于止咳宁嗽胶囊中活性组分绿原酸、金丝桃苷和橙皮苷含量的同时测定。     

多级梯度淋洗-抑制电导离子色谱法同时测定水中13种阴离子

建立了多级梯度淋洗-抑制电导离子色谱法测定水中13种阴离子的分析方法,通过对流速、柱温、pH、色谱柱选择、淋洗液浓度等影响因素的研究,探索出了适合13种阴离子分析测定的多级梯度淋洗条件。最优实验条件为:流速为1.00 m L/min,柱温为35℃,pH在5.6~6.9之间。实验结果表明,除CO~(2-)_3自身不稳定外,其他12种组分在0.005~20.0 mg/L质量浓度范围内具有良好的线性关系(0.9995),检出限(S/N=3)为0.8~16.0μg/L;在0.10,0.20,5.00 mg/L 3个添加浓度水平下,回收率在90.4%~107.6%之间,相对标准偏差为0.08%~5.3%。方法适于饮用水、地下水、灌溉水等环境水体中13种阴离子的痕量分析测定。     

高效液相色谱-蒸发光散射法测定牛黄中多种有效成分含量及其质量相关性研究

建立高效液相色谱-蒸发光散射法(HPLC-ELSD)同时快速测定牛黄中7种组分的含量的方法。色谱柱为UltimateAQ-C18柱,流动相为乙腈-0.2%甲酸水溶液,梯度洗脱,流速1mL/min;蒸发光散射检测器参数:漂移管温度100℃,载气(N2)流速1.9L/min。在选定色谱条件下,胆固醇、各种胆汁酸及其钠盐峰形良好且能达到很好地分离。各组分色谱峰峰面积的对数与浓度的对数呈良好线形关系(r0.9972);标准加入回收率为98.8%～112.7%;7种组分的最低检出限为0.001～0.007g/L。本方法可简便、快速地同时检测不同牛黄样品中7种组分的含量并可表征不同牛黄样品的质量,从而为该名贵药材的质量控制提供更全面的依据和参考。     

高效液相色谱法同时测定防晒类化妆品中二苯酮-2等3种防晒剂组分的含量

建立一种高效液相色谱法同时测定防晒类化妆品中3种防晒剂组分(二苯酮-2、二乙氨羟苯甲酰基苯甲酸己酯和二乙基己基丁酰胺基三嗪酮)的含量。色谱柱为Inertsil C_(18)(4.6×250 mm,5μm),流动相为甲醇-水,梯度洗脱,流速为1.0 mL/min,检测波长二苯酮-2为335 nm、二乙氨羟苯甲酰基苯甲酸己酯为356 nm、二乙基己基丁酰胺基三嗪酮为307 nm。3种新型防晒剂组分在40 min内完全分离,线性范围0.96~66.5 mg/L(r=0.999 8~0.999 9),检测限为0.01~0.04 mg/L,定量限为0.03~0.11 mg/L,回收率为98%~107%。该方法简便、快速、准确、可靠,适合防晒类化妆品中防晒剂组分的含量测定。     

反相高效液相色谱梯度洗脱同时测定复方茶碱片中7组分的含量

建立了一种灵敏、快速的反相高效液相色谱梯度洗脱方法，用于同时测定复方茶碱片中7组分的含量。采用YWG C18柱，以甲醇-磷酸二氢钠为流动相，用二极管阵列检测器，检测波长为214nm,15min即可将7种组分分离测定。该方法快速淮确，线性范围广，用于实际样品的测定，结果满意。     

反相高效液相色谱法测定C60衍生物[6,6]苯基C61-丁酸甲酯的含量

建立了一种反相高效液相色谱方法,分离C60、其衍生物[6,6]苯基C61-丁酸甲酯和[5,6]苯基C61-丁酸甲酯及二加成物,并测定其中[6,6]苯基C61-丁酸甲酯的含量。采用C18柱(3μm,2.1×100 mm),以V(CHCl3)∶V(乙腈)=30∶70溶剂为流动相,流量0.15 mL/min,柱温35℃,检测波长350 nm,25min内即可将各种组分分离。采用外标法测定其中[6,6]苯基C61-丁酸甲酯的含量。该方法快速、简便、准确,可用于定量分析[6,6]苯基C61-丁酸甲酯。     

梯度淋洗-电导抑制离子色谱法同时测定果汁中26种有机酸和阴离子

通过对色谱柱类型、流速、柱温、pH值、淋洗液浓度等影响因素的研究,建立了多级梯度淋洗-电导抑制离子色谱同时测定果汁中26种有机酸和阴离子的分析方法。结果表明,当流速为1.00 mL/min、柱温为30℃、pH值为5.5~6.8时,26种组分的测定结果更准确。26种组分在0.02~10.0 mg/L范围内具有良好的线性关系（r均大于0.995）,检出限（S/N=3）为0.17~52.0 μg/L;在0.20~2.00 mg/L添加水平下的回收率为85.58%~108.86%,相对标准偏差为0.15%~7.65%（n=6）。该方法简便快速、灵敏度好、准确度高,适于果汁中26种组分的痕量分析。     

气相色谱法测定茶叶中的噻嗪酮、甲胺磷、乙酰甲胺磷及三唑磷残留

建立了同时测定茶叶中噻嗪酮、甲胺磷、乙酰甲胺磷和三唑磷4种农药残留量的测定方法。在45 ℃加温条件下,用乙酸乙酯-正己烷混合溶剂提取及活性炭色谱柱净化,用不同配比的乙酸乙酯-正己烷混合液梯度洗脱待测组分,以DB-210毛细管色谱柱分离、氮磷检测器测定。结果表明,上述4种农药在10 min内能很好地分离;样品加标回收率(n=3)为73.4%~96.9%。方法的变异系数为2.49%~3.35%,茶叶（干重）中4种农药的定量检测下限为7.0~12.0 μg/kg。     

气相色谱法快速测定天然气中14种组分的含量

采用气相色谱法快速测定天然气中14种组分的含量。通过1次进样自动分流后,分别用4根微型色谱柱链接4个独立的热导检测器在5min内同时分离测定天然气中的甲烷、乙烷、丙烷、氮气、氧气、氦气、氢气、二氧化碳及丁烷、戊烷的同分异构体等组分。14种组分的浓度在一定范围内呈线性,检出限(3S/N)在11~19μmol·mol-1之间,测定值的相对标准偏差(n=8)小于1%。以标准物质GBW(E)061322对仪器进行校准,分析了四川地区的天然气中14种组分。     

代谢组学方法研究姜黄根茎及块根次生代谢产物表达差异

基于GC-MS的代谢组学分析方法,建立了分析不同产地来源的姜科植物姜黄( Curcuma.Longa L)的根茎(中药姜黄)和块根(中药郁金)的次生代谢产物的方法.对样品的提取方法、气相升温条件和方法学进行了考察,确定采用石油醚索氏提取法对样品进行提取.色谱图中主要化合物的精密度为1.2％～5.7％;重现性为2.18％～6.27％;回归系数R2=0.699～0.972.数据处理采用SIMCA P软件进行主成分(PCA)分析,通过主成分得分图( Score plot)可以明显区分姜黄的根茎及块根样品,说明在根茎和块根中次生代谢产物的表达存在差异;通过载荷图(Loading)和t检验(t-test)发现了14种表达差异显著的化合物.这些化合物可能是姜黄根茎与块根具有不同药性和临床用途的物质基础.     

气相色谱-质谱法测定姜黄挥发油化学成分

采用水蒸气蒸馏法提取姜黄挥发油,用气相色谱－质谱联用技术分离和鉴定姜黄挥发油的化学成分。经计算机ＮＢＳ谱库检索,发现姜黄挥发油中至少有１５个峰,鉴定出α－姜黄烯、α－姜烯、桉叶油素和球姜酮等１５种组分;另外还有１－（３－环戊基醛）－２,４－二甲基苯、β－倍半水芹烯、大根香叶酮、大根香叶烷、顺双环［３,３,１］酮－２－烯－９－醇等成分。姜黄挥发油中主要成分为α－姜黄烯。     

高效液相色谱-串联质谱法分析姜黄中微量的姜黄素类化合物

建立了同时检测中药姜黄中3种微量的姜黄素类化合物的高效液相色谱-电喷雾串联质谱分析方法。姜黄根茎经乙醇超声提取后,无需其他处理可直接进样分析。以Microsorb C18色谱柱(250 mm×4.6 mm,5 μm)分离,乙腈和0.1%甲酸水梯度洗脱,在多反应监测模式(MRM)下对目标成分进行定性分析。利用质谱碎裂规律,分别对每个目标成分同时监测8个母离子/特征子离子对的反应过程,首次从姜黄中发现了3个微量的姜黄素类化合物成分。一次性完成了目标成分的同时定性,方法的检出限为0.2 μg/L。结果表明,该方法具有简便、快速、准确、灵敏度高的优点,适用于中药复杂体系中姜黄素类化合物的分析检测。     

ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spectrometry.The results are consistent with those obtained by conventional steam distillation extraction method.The optimum condition of flash distillation has been studied.The experimental results showed that this new technique proved to be a simple,rapid and efficient tool for microanalysis of volatile constituents of Chinese medicinal herbs.     

闪蒸-毛细管气相色谱-质谱法分析中草药的挥发性成分

本文采用闪蒸-毛细管气相色谱-质谱法对姜黄、茅苍术、小茴香、肉桂的主要挥发性组分进行了分析,其结果与常规分析相符,对中草药闪蒸分析的条件进行了探讨,实验结果证明,闪蒸分析法是研究中草药挥发性成分的一种简便、快速、有效的微量分析方法。     

Spectroscopic studies on the molecular interactions of curcumin and piperine

Monatshefte für Chemie - Chemical Monthly - The diarylheptanoid curcumin is the yellow coloring agent accumulated in the rhizome of the common spice turmeric (Curcuma longa L.). It has...     

Antiradical efficiency of 20 selected medicinal plants

The antioxidant system of a plant comprises a group of chemicals that are highly diverse in their sources, effects and uses. These antioxidants are capable of contracting and damaging free radicals. This investigation deals with a screening and comparison of the antioxidant activities of 20 selected medicinal plants and their parts, individually and in combination with vitamins A, C or E, using the DPPH radical scavenging method. Phyllanthus emblica L., Santalum album L., Syzygium cumini L. and Trigonella foenum-graecum L. presented highly significant antiradical efficiency (AE) singly and in combination with either vitamin A, C or E. Further, Curcuma longa L., Momordica charantia L., S. cumini, T. foenum-graecum, Moringa oleifera Lam and S. album have also shown fairly significant AE in a vitamin combination dose of 0.001 mM concentration.     

Free radical scavenging activity and characterization of sesquiterpenoids in four species of Curcuma using a TLC bioautography assay and GC-MS analysis

The sesquiterpenoids are one of major groups of antioxidants in Curcuma besides curcuminoids. However, the real substances contributing to the antioxidant activity are still unknown. In this paper, the antioxidant activity of sesquiterpenoids in four species and two essential oils from Curcuma genus was determined and compared based on TLC separation and DPPH bioautography assay. Their antioxidant capacities were quantitatively evaluated using densitometry with detection at 530 nm (λ(reference )= 800 nm) using vitamin C as reference. The results showed that Curcuma longa rhizomes had the highest antioxidant capacity while C. phaeocaulis presented the lowest one among the four species of Curcuma. Moreover, essential oil of C. wenyujin showed higher antioxidant potential than that of C. longa. The main TLC bands with antioxidant activity of the four species of Curcuma were collected and characterized using GC-MS, and thus curzerene, furanodiene, α-turmerone, β-turmerone and β-sesquiphellandrene were determined as major sesquiterpenoids with antioxidant activity in Curcuma.     

Fast determination of curcumol, curdione and germacrone in three species of Curcuma rhizomes by microwave-assisted extraction followed by headspace solid-phase microextraction and gas chromatography-mass spectrometry

Curcumol, germacrone and curdione are the main active ingredients in a common traditional Chinese medicine (TCM) of Rhizoma Curcuma, and commonly used as the TCM quality control markers. In the present work, microwave-assisted extraction (MAE) followed by headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was developed for the quantitative analysis of curcumol, curdione and germacrone in Rhizoma Curcuma. The MAE and HS-SPME parameters were studied, and the method was validated. The optimal MAE conditions obtained were: microwave power of 700 W and irradiation time of 4 min, and HS-SPME optimal conditions were: fiber coating of 100 microm PDMS, extraction temperature of 80 degrees C, extraction time of 20 min, stirring rate of 1,100 rpm, and salt concentration of 30% NaCl. The proposed method provided good precision (RSD less than 12%) and recoveries between 86% and 93%. The proposed method was applied to the determination of the three marker compounds in three species of Curcuma rhizomes (Curcuma wenyujin, Curcuma phaeocaulis, and Curcuma kwangsiensis). To demonstrate the proposed method reliability, a conventional technique of steam distillation was also used for the analysis of curcumol, germacrone and curdione in the TCMs. The results show that MAE-HS-SPME is a simple, rapid, solvent-free and reliable method for the determination of curdione, curcumol and germacrone in TCM, and also a potential and powerful tool for quality assessment of Rhizoma Curcuma.     

The core structure of ukonan A, a phagocytosis-activating polysaccharide from the rhizome of Curcuma longa, and immunological activities of degradation products.

The controlled Smith degradation of ukonan A, a phagocytosis-activating polysaccharide isolated from the rhizome of Curcuma longa L., was performed. The reticuloendothelial system-potentiating, anti-complementary and alkaline phosphatase-inducing activities of ukonan A and its degradation products were investigated. Methylation analyses of both the primary and the secondary Smith degradation products indicated that the core structural features of ukonan A include a backbone chain mainly composed of beta-1,3-linked D-galactose, beta-1,4-linked D-xylose and alpha-1,2-linked L-rhamnose residues. All of the galactose units in the backbone carry side chains composed of alpha-L-arabino-beta-D-galactosyl or beta-D-galactosyl residues at position 6. Ukonan A has a remarkable effect on each of the three kinds of immunological activities. Periodate oxidation caused pronounced decrease or disappearance of the activities, but the controlled Smith degradation product having the core structure of polysaccharide showed considerable restoration of these activities.