大黄药材中大黄苷元含量测定

[目的]采用HPLC法测定不同产地的大黄药材中5种蒽醌苷元的含量。[方法]HPLC色谱条件为：色谱柱为Diamonsil C18柱（5μm,250.0 mm×4.6 mm）;流动相为甲醇-0.05%磷酸水溶液（V∶V=85∶15）;流速为1 ml/min;检测波长245 nm;进样量为20μl。[结果]大黄各苷元线性关系良好,平均回收率为97.55%～100.87%,RSD值为1.38%～2.47%。大黄药材中各苷元含量范围分别为：芦荟大黄素0.26%～0.52%,大黄酸0.21%～1.47%,大黄素0.26%～0.40%,大黄酚0.29%～1.95%,大黄素甲醚0.48%～2.72%。[结论]该方法精密度良好、重现性、稳定性好,适合大黄药材中各大黄苷元的质量控制。     

Effects of the aglycone of ascaulitoxin on amino acid metabolism in Lemna paucicostata

Ascaulitoxin and its aglycone (2,4,7-triamino-5-hydroxyoctanoic acid, CAS 212268-55-8) are potent phytotoxins produced by Ascochyta caulina, a plant pathogen being developed for biocontrol of weeds. The mode of action of this non-protein amino acid was studied on Lemna paucicostata. Ascaulitoxin is a potent growth inhibitor, with an I₅₀ for growth of less than 1 μM, almost completely inhibiting growth at about 3 μM. Its action is slow, starting with growth inhibition, followed by darker green fronds, and then chlorosis and death. Most amino acids, including non-toxic non-protein amino acids, reversed the effect of the toxin when supplemented in the same medium. Supplemental sucrose slightly increased the activity. d-Amino acids were equally good inhibitors of ascaulitoxin activity, indicating the amino acid effects may not be due to inhibition of amino acid synthesis. Oxaloacetate, the immediate precursor of aspartate, also reversed the activity. LC-MS did not detect interaction of the compound with lysine, an amino acid that strongly reversed the effect of the phytotoxin. Metabolite profiling revealed that the toxin caused distinct changes in amino acids. Reduction in alanine, paralleled by enhanced levels of the branched chain amino acids valine, leucine and isoleucine and nearly unchanged levels of pyruvate, might indicate that the conversion of pyruvate to alanine is affected by ascaulitoxin aglycone. In addition, reduced levels of glutamate/glutamine and aspartate/asparagine might suggest that synthesis and interconversion reactions of these amino group donors are affected. However, neither alanine aminotransferase nor alanine: glyoxylate aminotransferase were inhibited by the toxin in vitro. Our observations might be explained by three hypotheses: (1) the toxin inhibits one or more aminotransferases not examined, (2) ascaulitoxin aglycone affects amino acid transporters, (3) ascaulitoxin aglycone is a protoxin that is converted in vivo to an aminotransferase inhibitor.     

相溶解度法测定β-环糊精与4种黄酮类苷元的超分子包合常数

[目的]探讨β-环糊精促进黄酮类化合物色谱分离的可能性。[方法]以银杏黄酮中的4种苷元作为研究对象,研究β-环糊精对结构类似物在溶液条件下的包合作用,通过相溶解度法测定β-环糊精与不同黄酮苷元之间的相互作用。[结果]β-环糊精与槲皮素、木犀草素、山柰酚和异鼠李素的超分子包合常数分别为442.42、1 088.17、187.47、278.24 L/mol,说明β-环糊精可以高效选择性地结合一些黄酮,从而提高色谱分离度。[结论]β-环糊精可以尝试作为液相色谱流动相添加剂使用,提高不同黄酮苷元之间的分离度。     

茶叶中游离态和键合态香气组分对茶云纹叶枯病致病菌的抑制作用

从茶鲜叶中提取糖苷类物质,用茶叶粗酶水解后气相色谱分析挥发性酶解产物.结果表明顺-3-己烯醇、芳樟醇氧化物、芳樟醇、水杨酸甲酯、香叶醇、苯甲醇和苯乙醇是水解后挥发性苷元的主要成分,且挥发性苷元含量远高于相应的游离态香气;茶叶游离态香气组分和键合态糖苷类香气前体对茶云纹叶枯病致病菌均具有显著的抑制作用.抗菌试验结果表明,当茶叶游离态香气组分为0.5～2.5 μL·L-1时,其对茶云纹叶枯病致病菌具有不同程度的抑制作用,其中香叶醇抑制作用最强,最小抑制浓度(MIC)为0.5 μL·L-1;当茶叶键合态糖苷类香气前体质量浓度为5～25 mg·mL-1时,其对茶云纹叶枯病致病菌也具有显著的抑制作用.     

沙棘叶中黄酮糖苷和黄酮配基的含量

本文对沙棘叶分别用甲醇和乙醇(70%)进行了提取和盐酸催化的水解实验,采用HPLC方法测定了提取液和水解液中的黄酮配基含量.实验证明:用甲醇在回流温度下提取4h,每克叶仅得到槲皮素0.003mg,无山奈素和异鼠李素.用盐酸对叶水解3h,每克叶子能得到槲皮素1.562mg,山奈素1.496mg,异鼠李素2.398mg.叶提取的槲皮素仅是叶水解得到的0.2%.由此可见,沙棘叶中的黄酮配基是以黄酮糖苷的形式存在,在水解过程中可由糖苷经水解反应形成,对槲皮素、山奈素和异鼠李素都是如此.     

Bioactivity and chemical components of Thai rice in five stages of grain development

Tracking changes in the bioactive compounds of white (ML-W), red (ML-R) and black (RB) rice during the 5 stages of grain development were studied. Total anthocyanin (TAC) was found only in RB (stages 3–5) and proanthocyanidin (TPAC) contents were only found in ML-R (stages 2–5). Considerable amounts of total phenolic contents (TPC) were found in stages 2–4 of ML-R, while total flavonoid contents (TFC) were most detected in stages 4–5 of RB. The DPPH activity of ML-W and ML-R decreased from stages 1–5. The highest FRAP activity was found in ML-R (stages 2–3) indicating that it is highly related to the bioactive compound content. Cyanidin-3-glucoside and peonidin-3-glucoside were found in RB at stages 3–5. The cyanidin of RB in stages 4–5 was related to the amount of TAC. The proanthocyanidin compound catechin was first found and reported in stages 2–3 of ML-R. Principal component analysis indicated that antioxidant activity and the bioactive components were highly related. The data from this study suggests that ML-R at stage 2 and RB at stage 4 are the most suitable stages for harvesting to achieve the highest level of bioactive compounds, which have many health benefits.     

β-葡萄糖苷酶水解银杏黄酮糖苷的研究

采用β-葡萄糖苷酶水解银杏叶提取物(GBE),使糖苷型黄酮转化为苷元型黄酮。通过正交试验得出水解的最佳工艺参数,即温度40℃,酶浓度5×10-3mg/ml,pH值5.0下水解6 h。由HPLC图谱可得该条件下水解的苷元得率9.08%,纯度68.24%。酶解产物中还部分保留了银杏内酯等活性成分,有利于保留银杏叶提取物的综合生物活性。     

发酵处理对毛豆异黄酮苷元含量及其乙醇提取物抗氧化活性的影响

【目的】测定毛豆、发酵处理毛豆和大豆中的大豆苷元、黄豆黄素与染料木素3种异黄酮苷元以及多酚类化合物的总含量,并分析其乙醇提取物的抗氧化活性。【方法】利用回流法酸水解样品中的大豆异黄酮,通过高效液相色谱法测定大豆苷元、黄豆黄素和染料木素的含量;利用福林酚法测定3种样品中的多酚类物质总含量,并通过测定清除DPPH自由基、ABTS自由基和还原力比较样品乙醇提取物的抗氧化活性。【结果】毛豆、发酵处理毛豆和大豆的大豆苷元含量分别为255.96,286.04和358.08μg/g,黄豆黄素含量分别为57.96,65.51和59.73μg/g,染料木素含量分别为12.88,26.40和4.62μg/g。发酵处理毛豆中染料木素含量增加明显,分别为毛豆和大豆染料木素含量的2.05和5.71倍。发酵处理毛豆、大豆、毛豆中的多酚类化合物总含量分别为(3.31±0.138)mg/g、(1.148±0.028)mg/g和(2.69±0.011)mg/g,发酵处理毛豆的多酚类化合物含量约是大豆和毛豆的2.9和1.2倍。抗氧化活性比较表明,发酵处理毛豆清除ABTS自由基与DPPH自由基的能力优于大豆和毛豆。发酵处理毛豆、大豆和毛豆还原力大小依次表现为发酵处理毛豆毛豆大豆。【结论】经过发酵处理后,毛豆中的3种异黄酮含量均有所增加,但以染料木素的增加最为明显;发酵处理毛豆中多酚类化合物总含量升高,自由基清除活性增强。     

Philinopgenin A,B, and C,Three New Triterpenoid Aglycones from the Sea Cucumber Pentacta quadrangulasis

Three new triterpenoid aglycones named Philinopgenin A (1), B (2), and C (3) were isolated from the acid hydrolysate of the crude glycoside mixture prepared from the whole sea cucumber Pentacta quadrangulasis Lesson. The corresponding structures were determined as 16β-acetoxyholosta-8(9), 24(25)-diene-3β-ol (1), 20, 25-epoxy-lanosta-9(11)-ene-3β-ol 18(16)–lactone (2) and 16β-acetoxyholosta-9(11), 24(25)-diene-3β-ol (3), respectively, on the basis of spectral evidence.