大孔吸附树脂分离纯化龙胆药材中龙胆苦苷和马钱子苷酸的研究

目的:建立利用大孔吸附树脂对龙胆药材中龙胆苦苷和马钱子苷酸进行富集和分离纯化的方法。方法:采用加速溶剂萃取法对龙胆药材中两种有效成分进行高效提取,比较了D301,AB-8,D101,XDA-1四种大孔树脂对龙胆苦苷和马钱子苷酸的吸附性能,最终确定采用D301型大孔对脂对二者进行富集吸附,对其工艺参数进行优化,全程采用高效液相色谱进行目标化合物浓度检测。结果:化优后的工艺参数为:上样浓度:0.2 g/mL,最大上样量:0.25 g龙胆药材/g树脂,最佳静态吸附时间:8 h,采用8%和55%的乙醇溶液对龙胆苦苷和马钱子苷酸分别进行洗脱;龙胆苦苷和马钱子苷酸分别富集在8%和55%的乙醇洗脱液中,洗脱液浓缩后冷冻干燥,可得到纯度分别为74.3%和80.9%的粗产物,龙胆苦苷和马钱子苷酸的回收率分别为70.11%和67.82%。结论:此法效率较高,操作简便,即可用于实验室制备少量的难以购置的标准品,也可进行放大研究,用于工业生产。国家自然科学基金重点项目(20235020);; 青岛“2004将才计划”(04-3-JJ-11);; 共建生物医药研发测试中心(LS-05-KJZX-76)资

Content of gentiopicroside and loganic acid in Radix gentianae and their fingerprints

To develop a HPLC-DAD-ESI-TOF/MS analysis method for the determination of gentiopicroside and loganic acid in Radix gentianae samples and for the research of their fingerprints.The samples were extracted using ASE for 10 min under 100 ℃ and 9.65 MPa,and divided into water phase and chloroform phase and analyzed them with HPLC-DAD-ESI-TOF/MS method respectively.Based on this method,the HPLC fingerprints of Radix gentianae were established.Comparing the spectrogram and mass spectrum of the chromatogram peak with the reference value,three compounds in water phase were identified as gentiopicroside,asafetida acid and loganic acid.There is no report of the compounds in chloroform phase.The content of gentiopicroside and loganic acid in samples of different groups were determined,separately.The fingerprints were compared by the software of the similarity evaluation system for chromatographic fingerprint.The water phase fingerprint congruence coefficients of samples from six different areas were above 0.90,however,the chloroform phase fingerprint congruence coefficients were within 0.62-0.99.This method can be used for determination of potent component in Radix gentianae and its quality control.Radix gentianae from different producing areas have the largest diversities,and the diversities embodied in the content of chloroform phase compounds.青岛“2004将才计划”(04-3-JJ-11);; 国家海洋局青年基金资助项目(2005602);; 崂山区政府区校共建生物医药研发测试中心资助(LS-05-KJZX-76)

Determination of Gentiopicroside and Loganic Acid in Radix Gentianae by MEKC and MEEKC Mode

目的建立胶束电动毛细管色谱(MEKC)和微乳液毛细管电动色谱(MEEKC)分析龙胆药材中龙胆苦苷和马钱子苷酸含量的方法。方法采用加速溶剂萃取法(ASE)对龙胆药材进行提取,萃取温度:100℃,压力:9.65MPa,萃取时间:10min。采用未涂层熔融石英毛细管(内径75μm,有效长度50cm)。分别考察了两种分离模式下电泳介质的构成和电泳过程中的各操作参数对样品分离过程的影响,优化了MEKC和MEEKC的分析条件,在各自对应的缓冲液体系下,MEKC和MEEKC分离电压分别为30和22kV,柱温均为25℃,检测波长均为238nm。结果在选定的工作条件下,龙胆苦苷和马钱子苷酸与其他组分达到了基线分离,两种成分的浓度与其响应信号值之间具有较好的线性相关性,加标回收率在96.3%～105.1%之间,检测限均低于10mg·L-1,对6处不同产地的龙胆药材进行了分析,并对测定结果进行了t检验,结果表明,两种模式下,测定结果之间不存在显著性差异,而不同产地的龙胆药材的龙胆苦苷和马钱子苷酸含量之间存在较大差异。结论本方法简便,准确,快速,重现性较好,可用于龙胆药材有效成分的含量测定和质量控制。OBJECTIVE To develop MEKC and MEEKC modes for the determination of gentiopicroside and loganic acid in extracts of Radix Gentianae. METHODS The analyte was extracted from Radix Gentianae samples by accelerated solvent extraction, and the extraction conditions were optimized. Separation and determination were carried out on a bared fused silica capillary(50 cm×75 μm) with corresponding buffer. The run voltage of MEKC and MEEKC were 30kV and 22 kV respectively. Detection wavelength of DAD was at 238 nm and column temperature was 25 ℃. RESULTS The developed ASE-HPCE method was simple and reliable for the determination of gentiopicroside and loganic acid in Radix Gentianae samples with a broad linear dynamic range, a recovery range of 96.3%～105.16%,and the detection limit was below 10 mg·L-1. The contents of gentiopicroside and loganic acid in six samples from different regions were determined by the developed method in two modes. T-test value indicated that the determined contents of gentiopicroside and loganic acid by MEKC and MEEKC were consistent. CONCLUSION The method is simple,accurate,rapid and with good reproducibility.It can be used to determine active components in Radix Gentianae.国家自然科学基金重点项目(20235020);; 青岛“2004将才计划”(04-3-JJ-11);; 崂山区校区共建生物医药研发测试中心资助(LS-05-KJZX-76

紙品在休閒事業上之應用

The utilization of paper in leisure industry depends on the strength, water resistance, air resistance and grease resistance, softness of paper products. High tensile, fold endurance and water/grease resistance of paper fibers can be used as food packagin紙品在休閒事業上之應用視紙力、抗水性、抗透氣性、抗油性及衛生紙類之柔軟度而用途迥異。食品包裝紙類之紙纖維之高拉力∕耐折力為共同特性，雖然紙力可藉抄紙成形時之纖維交織加以控制，但其抗水性及乾∕濕強性尚須藉化學藥品之添加方為功。這些化學添加物可賦予紙張平滑度、印墨吸收性，外觀性及抗水性等功能。藉著塗佈技術提升紙之印刷適性及改善紙之表面平滑度可用於休閒業之包裝及廣告用途。塗佈紙及一般白紙可裝筷子。手感衛生紙之柔軟度、白度及吸水性為衛生紙類之重要性質。抗水蒸氣性如同紙力為速食店慣用之紙便當盒（或食品盒）之主要性

保水剂对梭梭（Haloxylon ammodendron）、白梭梭（Haloxylon persicum）种子萌发及幼苗根系的影响/Effect of Super Absorbent Polymer on Seed Germination and Seedling Roots of Haloxylon ammodendron and H. persicum[J]

在盆栽条件下,研究保水剂对梭梭（Haloxylon ammodendron）、白梭梭（Haloxylon persicum）种子萌发和幼苗根系形态的影响。结果表明：0.05%浓度的保水剂对梭梭、白梭梭种子萌发有明显的促进作用,发芽率较对照分别提高了18.7%和24.0%;0.05%浓度的保水剂能够抑制梭梭幼苗根系的垂直生长,有效促进侧根数量的增加和根系生物量的积累;0.1%浓度保水剂处理下,白梭梭的主根长度、侧根数量、根系生物量均达到最大;保水剂浓度达到0.2%时,梭梭、白梭梭种子萌发和幼苗根系的生长均受到抑制,表明梭梭幼苗生长最适宜的保水剂浓度为0.05%,白梭梭的浓度以0.05%～0.1%为宜

不同坡向梭梭幼苗的生长状况和适应特征/Growth and Adaptation of Haloxylon ammodendron Seedlings in Different Habitats in Guerbantunggut Desert[J]

以古尔班通古特沙漠南缘一年生梭梭移栽苗为研究对象,对梭梭幼苗的地上部分生长状况、蒸腾速率日变化趋势以及根系形态进行了调查,探讨不同坡向梭梭幼苗的生长和适应特征.结果表明,平地、阴坡和阳坡表层0～30 cm土壤含水量无显著差异,40～100 cm土壤含水量阳坡＜阴坡＜平地.梭梭幼苗同化枝生长速率和含水量均表现为阳坡＜阴坡＜平地,其生长速率和含水量可能与根层土壤含水量高低有关.不同坡向梭梭幼苗蒸腾速率日变化均呈“单峰型”,12:00-16:00阳坡梭梭幼苗蒸腾速率显著高于阴坡与平地.阳坡梭梭幼苗主根不发达,侧根较多但较短；平地和阴坡梭梭幼苗根系主根发达,以单根为主.这反映出根系对相应生境下土壤水分的适应特征