分别使用正相柱和反相柱,采用高效液相色谱‐紫外检测器( high performance liquid chromatography‐ultraviolet detector , HPLC‐UV)法测定植物甾醇,比较2种色谱柱法对植物甾醇检测的优缺点.正相色谱条件为:以Hypersil SiO2(4.6 mm ×250 mm ,5μm)为色谱柱,流动相为V (正己烷)∶V (异丙醇)=99∶1,柱温35℃,流速1.0 mL/min ,检测波长205 nm ;反相色谱条件为:以默克 RP‐18(4.6 mm ×250 mm ,5μm)为色谱柱,流动相为纯甲醇,柱温35℃,流速1.0 mL/min ,检测波长205 nm .结果表明:混合甾醇在反相柱分离下出现3个峰,各种甾醇的分离度好;正相柱的甾醇只有1个峰,但样品在正相体系中的溶解性高于反相体系,而且正相体系甾醇出峰时间比反相体系快,可节约实验时间.说明在不要求各种甾醇分离效果的前提下,正相柱更适合用于植物甾醇检测.

@@@@Summary Phytosterols are natural bioactive compounds , usually including stigmasterol , sitosterol , campesterol , and rapeseed sterol . They have attracted growing attention owing to their beneficial effects . High performance liquid chromatography ( HPLC ) is the most frequently used method to quantify phytosterols . Although several detectors such as ELSD ( evaporative light scattering detector) and UV ( ultraviolet detector) are available for HPLC analysis , but UV detector is believed to be much more effective and always preferred in laboratories . In the recent literature available , the reverse phase column was mostly applied to determine phytosterols in HPLC‐UV system . However , the performance of normal phase column in phytosterol analysis has not been well studied and compared . In this study , the performances of both reverse phase and normal phase columns in HPLC‐UV system for phytosterol analysis were compared , and their respective advantages were illustr

建立正相高效液相色谱法测定花生油中的维生素E组分的方法。花生油中维生素E用正己烷直接提取后采用正相高效液相色谱法,荧光检测器检测。维生素E各组分浓度在0.01~100g/m L峰面积与含量具有良好的线性关系,平均相对标准偏差在0.47%~0.92%,平均回收率为94.9%~98.7%。该方法快速,准确,灵敏度高,可作为花生油中维生素E含量测定的检测方法。

A normal-phase high performance liquid chromatography method was developed for determination of vitamin E components in peanut oil. Vitamin E components in peanut oil samples were extracted by n-hexane, and then determined by normal-phase high performance liquid chromatography with fluorescence detection. Results showed that 0.01~100 g/mL vitamin E components and peak areas were of good linear relationship. Average relative standard deviations were 0.47%~0.92%and average spike recoveries were 94.9%~98.7%. This method demonstrated to be simple and accu-rate with high precision, and thus had a promising potential for the determination of vitamin E in peanut oil.

以淫羊藿提取物为原料,通过正相硅胶柱色谱和凝胶柱色谱等分离纯化手段,研制了宝藿苷Ι纯度标准物质。采用液相色谱–质谱法和核磁共振技术对宝藿苷Ⅰ纯度标准物质进行定性鉴定,利用高效液相色谱(HPLC)法和胶束电动毛细管色谱(MECC)法对宝藿苷Ι的纯度进行定值分析,同时利用HPLC法对宝藿苷Ι纯度标准物质进行均匀性检验与稳定性考察,通过F检验和t检验法对其均匀性进行检验,表明瓶间和瓶内均匀性一致,12个月稳定性检验结果的相对标准偏差为0.02%,说明宝藿苷Ι纯度标准物质是稳定的。对定值结果的不确定度进行了评价,研制的宝藿苷Ι纯度标准物质的定值结果和扩展不确定度分别为99.7%和0.3%(k=2)。

BaohuosideⅠwas extracted from the leaves of epimedium brevicornu maxim, the extract was isolated by silica gel column chromatography and was purified further over Sephadex LH-20 column chromatography, and BaohuosideⅠpurity certified reference material(CRM)was presented. The qualitative analysis of BaohuosideⅠpurity CRM material was performed by high performance liquid chromatography-mass spectrometry(HPLC-MS)and nuclear magnetic resonance(NMR). The purity of Baohuoside Ⅰwas determined by high performance liquid chromatography(HPLC) and micellar electrokinetic capillary chromatography(MECC). Homogeneity and stability monitoring of Baohuoside Ⅰpurity CRM were performed by HPLC. Homogeneity was evaluated by F-test and t-test, the stability was monitored over 12 month, and the RSD of stability was 0.02%. The uncertainty evaluation was studied extensively. The certified purity value of BaohuosideⅠpurity CRM was 99.7%with expanded uncertainty of 0.3%(k=2).

对采自钦州湾的红树植物桐花树叶中分离得到的一株内生真菌ME-3的次生代谢产物的化学成分进行了研究。利用马铃薯葡萄糖液体培养基培养、乙酸乙酯萃取得到桐花树内生真菌ME-3的发酵液粗提物，采用正相硅胶柱色谱、反相硅胶柱色谱、葡聚糖凝胶SephadexLH-20柱色谱、制备薄层色谱和重结晶等方法对粗提物进行分离纯化，并运用现代波谱技术结合文献对照鉴定化合物结构。结果表明，从桐花树内生真菌ME-3的次代谢产物中分离获得3个化合物，根据它们的理化性质和波谱数据鉴定为：东莨菪内酯、邻苯二甲酸二丁酯和苯甲酸。其中，东莨菪内酯和苯甲酸为首次从桐花树内生真菌中发现。

The research aims to study the chemical constituents of endophytic fungus ME-3 which is isolated from the fresh leaf of marine-mangrove plant “Aegiceras corniculatum” picked in Qinzhou Bay. Three compounds have been isolated by a com-bination of silica gel, SephadexLH-20 and recrystallization approaches as well as the preparative thin layer chromatography. One is dibutylo-phthalate ester, the other two are scopoletin and benzoic acid which are found in the Aegiceras corniculatum endophyt-ic fungi for the first time.

采用正相、反相硅胶柱色谱法和半制备型高效液相色谱法对藤黄树脂的化学成分进行了分离和纯化,获得了5个化合物,通过NMR谱鉴定其结构分别为2α-羟基-3β-乙酰氧基白桦酯酸(I),2-O-乙酰基-山楂酸(II),邻苯二甲酸二丁酯(III),邻苯二甲酸二异丁酯(IV),邻苯二甲酸-二-2-乙基己酯(V),化合物2～5为首次从该植物中分离.

Five compounds were isolated from the resin of Garcinia hanburyi Hook. f. by silica gel, reversed-phase silica gel column chromatography and semi-preparative high performance liquid chromatography. The structures were identified as 2α-hydroxy-3β-acetoxy-lup-20(29)-en-28-oic acid (I), 2-O-acetylmaslinic acid (II), dibutyl phthalate (III), diisobutyl phthalate (IV) and bis(2-ethylhexyl)phthalate (V) by NMR spectroscopy. Compounds 2~5 were obtained from the plant for the first time.