延胡索标准汤剂研究

目的:制备延胡索标准汤剂,并进行质量标准研究。方法:药材经DNA分子鉴定为延胡索Corydalis yanhusuo W.T.Wang的干燥块茎。采用饮用水煎煮2次制备延胡索标准汤剂,考察延胡索标准汤剂特征图谱及延胡索乙素含量测定方法,并分别计算延胡索标准汤剂的出膏率、延胡索乙素含量及含量转移率,测定15批延胡索标准汤剂特征图谱。结果:15批延胡索标准汤剂出膏率为14.5%~32.5%;延胡索乙素含量为0.10%~0.24%;延胡索乙素含量转移率为30.7%~71.1%;对15批延胡索标准汤剂进行特征图谱测定,确定了9个共有峰,通过对照品指认4个色谱峰。结论:该方法中延胡索标准汤剂制备方法规范,样品质量稳定,方法精密度、稳定性、重复性良好,可为延胡索标配方颗粒质量标准建立提供参考。     

川芎地上部位的质量评价

目的:基于指纹图谱和含量测定对川芎地上部位(茎叶)进行质量评价。方法:采用Kromasil C18色谱柱(250mm×4.6mm,5μm),以0.1%磷酸水溶液(A)-乙腈(B)为流动相,梯度洗脱,流速:1.0mL/min,进样量20μL,柱温35℃,检测波长254nm,建立HPLC指纹图谱;采用Kromasil C18色谱柱(250mm×4.6mm,5μm),以水(A)-甲醇(B)(34∶66)为流动相,等度洗脱,流速:1.0mL/min,进样量10μL,柱温35℃,330nm和237nm双波长测定藁本内酯和丁烯基苯酞的含量。结果:建立了13批川芎地上部位的HPLC指纹图谱,标定了20个共有峰,指纹图谱相似度在0.89以上;13批样品中藁本内酯和丁烯基苯酞的含量分别为0.0642%~0.2633%和0.0057%~0.0325%。结论:该方法操作简便,结果准确,重现性好,可以为川芎地上部位的质量评价和质量控制提供参考。     

滇重楼地上部分总皂苷HPLC指纹图谱

目的:建立滇重楼地上部分总皂苷高效液相色谱法(HPLC)指纹图谱,为滇重楼地上部分总皂苷的质量控制提供参考。方法:采用Ecosil HPLC C₁₈色谱柱(250 mm×4.6 mm,5μm)进行分离,流动相为乙腈-水溶液,梯度洗脱,流速为1.0 mL·min^-1,检测波长为203 nm,柱温为31℃。建立6批滇重楼地上部分总皂苷HPLC特征图谱,并进行相似度评价;采用硅胶、反向硅胶RP-C₁₈柱色谱等方法对特征图谱中的3个未知共有峰化合物进行分离,应用质谱法(MS)、核磁共振(NMR)等方法进行结构鉴定;参照各对照品的色谱行为及其二极管阵列检测器(DAD)紫外光谱图,对共有峰进行归属和指认。结果:指纹图谱中的3个未知共有峰化合物为偏诺皂苷元-3-O-α-L-吡喃鼠李糖基-(1→4)-[α-L-吡喃鼠李糖基-(1→4)-β-D-吡喃葡萄糖苷(cld01)、偏诺皂苷元-3-O-α-L-吡喃鼠李糖基-(1→4)-β-D-吡喃葡萄糖苷(cld02)、薯蓣皂苷元-3-O-α-L-吡喃鼠李糖基-(1→4)-[α-L-吡喃鼠李糖基-(1→4)-β-D-吡喃葡萄糖苷(cld03)。cld02为首次从该植物中分离得到,cld03为首次从该植物地上部分分离得到;6批样品特征图谱与对照图谱的相似度均大于0.99,共归属指认了7个共有峰。结论:所建立的HPLC指纹图谱方法稳定、可靠、重复性好,可为滇重楼地上部分总皂苷质量控制提供参考。     

Treatment of Lesch–Nyhan disease with S-adenosylmethionine: Experience with five young Malaysians,including a girl

Background: Lesch–Nyhan disease (LND) is a rare X-linked recessive neurogenetic disorder caused by deficiency of the purine salvage enzyme hypoxanthine phosphoribosyltransferase (HPRT, EC 2.4.2.8) which is responsible for recycling purine bases into purine nucleotides. Affected individuals have hyperuricemia leading to gout and urolithiasis, accompanied by a characteristic severe neurobehavioural phenotype with compulsive self-mutilation, extrapyramidal motor disturbances and cognitive impairment. Aim: For its theoretical therapeutic potential to replenish the brain purine nucleotide pool, oral supplementation with S-adenosylmethionine (SAMe) was trialed in 5 Malaysian children with LND, comprising 4 related Malay children from 2 families, including an LND girl, and a Chinese Malaysian boy. Results: Dramatic reductions of self-injury and aggressive behaviour, as well as a milder reduction of dystonia, were observed in all 5 patients. Other LND neurological symptoms did not improve during SAMe therapy. Discussion: Molecular mechanisms proposed for LND neuropathology include GTP depletion in the brain leading to impaired dopamine synthesis, dysfunction of G-protein-mediated signal transduction, and defective developmental programming of dopamine neurons. The improvement of our LND patients on SAMe, particularly the hallmark self-injurious behaviour, echoed clinical progress reported with another purine nucleotide depletion disorder, Arts Syndrome, but contrasted lack of benefit with the purine disorder adenylosuccinate lyase deficiency. This first report of a trial of SAMe therapy in LND children showed remarkably encouraging results that warrant larger studies.     

微量盐酸可乐定含量测定

目的：建立高效液相色谱法测定微量盐酸可乐定的含量的方法。方法：色谱柱：C18柱，流动相：0．22％辛烷磺酸钠-甲醇-磷酸（500：500：1），用2mol／L氨水溶液调节pH至3.0；检测波长：220nm．外标法。结果：该方法的线性范围是101μg／ml～50μg/ml，R=0．9999；平均回收率为99．7％。RSD（％）=0．13％。结论：该方法测定样品效果佳，灵敏度高，结果准确可靠。     

蒲黄药材中香蒲新苷和异鼠李素-3-O-新橙皮苷含量测定方法优化研究

目的建立蒲黄中香蒲新苷和异鼠李素-3-O-新橙皮苷的含量测定方法。方法采用单因素考察方法建立供试品溶液制备方法;采用高效液相色谱法(HPLC)法测定香蒲新苷和异鼠李素-3-O-新橙皮苷的含量,色谱条件为Waters SunFire~(TM)C_(18)(4.6 mm×250 mm,5μm)色谱柱,乙腈-0.05%磷酸溶液梯度洗脱,流速1.0 m L/min,检测波长254 nm,柱温20℃。结果蒲黄药材采用80倍量的甲醇回流提取1.5 h,制备供试品溶液;香蒲新苷在0.245 2~1.471 0μg范围内线性关系良好,r=0.999 9,平均加样回收率为98.47%,相对标准偏差(RSD)=2.05%(n=6);异鼠李素-3-O-新橙皮苷在0.191 2~1.147 4μg范围内线性关系良好,r=0.999 7,平均加样回收率为100.56%,RSD=2.56%(n=6)。结论所建立的含量测定方法简便准确,重现性好,为蒲黄药材质量控制和评价奠定基础。     

高效液相色谱法建立黄芪多糖特征图谱研究

目的 探讨高效液相色谱法建立黄芪多糖特征图谱.方法 利用高效液相色谱法对PMP柱前衍生化的黄芪多糖进行糖组成分析.结果 黄芪多糖特定图谱由鼠李糖、葡萄糖、半乳糖、阿拉伯糖4种单糖4个共有峰组成.结论 高效液相色谱法建立的黄芪多糖特征图谱,其操作方法简便,具有良好的重复性及稳定性,可有效控制黄芪多糖的内在质量.     

HPLC法测定酵母菌细胞内维生素B1含量

目的 建立酵母菌细胞内维生素B1的含量测定方法.方法 采用Thermo DBS-C18分析柱(250 mm×4.6mm,5 μm),流动相为水-甲醇(70∶30),流速1.2 mL/min,柱温35℃,检测波长为238nm.结果 维生素B1在浓度1.0 ～ 5.0 μg/mL浓度范围内线性关系良好(y=294 400.5 X-65 837.9,r=0.997 9),方法回收率为88％ ～92％,重现性在RSD =0.8％～1.24％ (n =5).结论 本测定方法准确、可靠,重复性好,可用于测定酵母菌细胞内维生素B1含量.     

Phenolic composition of fruits from different cultivars of red and black raspberries grown in Poland

Fruits of 11 varieties of Rubus idaeus and 1 variety of Rubus occidentalis cultivated in Poland, were analyzed in terms of phenolic composition. The qualitative and quantitative determination of phenolics was performed by means of HPLC-DAD coupled with ESI–MS detector. Quantitative determination of anthocyanins, revealed significant differences in the levels of major anthocyanins in most red raspberry varieties, of which cyanidin 3-O-sophoroside was the most prevalent one. Black raspberries displayed 4–11 times more anthocyanin content compared to red raspberries, with the dominating anthocyanins being cyanidin 3-O-rutinoside and cyanidin 3-O-xylosyl-rutinoside.Sanguiin H-6 was the main ellagitannin identified in all varieties, with ‘Beskid’, ‘Laszka’, ‘Polana’ and ‘Litacz’ standing out as the richest sources of sanguiin H-6. Ellagic acid was at similar, low concentrations, with the highest levels observed in ‘Willamette’. A number of other compounds belonging to flavonols, flavan-3-ols and phenolic acids, were found at much lower levels than anthocyanins and ellagitannins, with the presence of procyanidins B₁ and B₂ being reported for the first time in the fruits of black raspberries. Data obtained on the variation in content of major and minor phenolic compounds between raspberry varieties highlights the most valuable cultivars to be used as a dietary source of phenolic compounds.     

HPLC法测定不同采收期承德产山里红叶牡荆素-4″-O-葡萄糖苷的含量

目的：采用高效液相色谱(HPLC）法测定承德地区不同采收期山里红叶中牡荆素-4″-O-葡萄糖苷的含量。方法：色谱柱为Agilent ZORBAX SB-C18(4.6mm×250mm,5μm）;流动相：0.1%甲酸水溶液-乙腈-四氢呋喃溶液,梯度洗脱;检测波长：340nm;流速1.0ml/min;柱温30℃。结果：牡荆素-4″-O-葡萄糖苷的线性范围是0.001-0.16mg/ml;平均加样回收率为100.2%(RSD=2.8%）;5-10月承德不同产地山里红叶中牡荆素-4″-O-葡萄糖苷的含量均值分别为滦平县3.00mg/g,双桥区4.00mg/g,承德县2.84mg/g。结论：承德地区山里红叶中牡荆素-4″-O-葡萄糖苷的含量在8月份达到最高,为最佳采收期,以承德市双桥区产的山里红叶含量最高,为最佳产地。