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1.
采用反相高效液相色谱法同时测定柚皮中柚皮甙和橙皮甙的含量。色谱条件:μ-BondapakC18柱(250mm×4.6mm,5μm),流动相为甲醇-0.5%乙酸溶液(V/V=38/62);流速为0.8mL·min-1;检测波长为283nm,柱温为25℃。柚皮甙和橙皮甙的线性范围分别为20-60mg·L-1和10-30mg·L-1。柚皮甙和橙皮甙的平均回收率分别为99.3%和97.8%。该方法具有快速,结果准确等优点。  相似文献   

2.
采用自制的苯氨基甲酸酯衍生化β-环糊精键合SBA-15手性固定相,以甲醇-水作流动相,拆分了柚皮甙对映体;考察了流动相组成、柱温、检测波长等对柚皮甙拆分和测定的影响,优化的色谱条件为:流动相为甲醇-水(55:45,V/V),流速0.5 m L/min,柱温20℃,进样量10μL,检测波长为285 nm。基于上述条件,对中草药化橘红、香橼、枳壳及柚皮中的柚皮甙对映体进行了含量测定。柚皮甙每个对映异构体均在0.5~500μg/m L范围内线性关系良好(r≥0.995),检出限为0.04μg/m L(S/N=3)。以化橘红为例,柚皮甙第一个对映体的加标平均回收率为93.8%和RSD为1.2%(n=5),第二个对映体的加标平均回收率为91.3%和RSD为1.6%(n=5)。测得化橘红、香橼、枳壳和柚皮中柚皮甙两对映体的含量分别为10.42 mg/g和15.84 mg/g,15.39 mg/g和49.52 mg/g,16.53 mg/g和95.80 mg/g,18.47 mg/g和30.98 mg/g。  相似文献   

3.
高效液相法测定注射用赖氨匹林中的阿司匹林及游离水杨酸   总被引:11,自引:0,他引:11  
董煜  赵远征  张怡娜 《色谱》2002,20(3):277-278
 建立了高效液相法 (HPLC)同时测定注射用赖氨匹林中阿司匹林和游离水杨酸含量的方法。采用的柱为HypersilBDSC18柱 ,流动相为甲醇 水 冰醋酸 (体积比为 35∶6 5∶3) ,检测波长为 2 80nm。阿司匹林和水杨酸的质量浓度分别为 0 0 2 8g/L~ 0 14 1g/L和 0 77mg/L~ 3 85mg/L时线性关系良好 ,其线性相关系数分别为0 9999和 0 9998;加样回收率分别为 99 2 7% (RSD =0 8% )及 99 6 1% (RSD =1 3% )。  相似文献   

4.
通过优化缓冲溶液pH和浓度、分离电压和进样时间等条件,建立了橙皮甙、柚皮甙、橙皮素和柚皮甙元4种物质的毛细管电泳分离分析方法.在优化的条件下10 min内实现了4种物质的毛细管电泳分离.橙皮甙、柚皮甙、橙皮素和柚皮甙元4种物质分别在0.03~0.80、0.03~0.85,0.02~0.60和0.02~0.65mg/mL浓度范围内和峰电流成线性关系,检出限分别为0.007、0.006、0.004和0.005 mg/mL.方法用于分析模拟样品得到满意的结果,有望用于实际样品分析.  相似文献   

5.
徐颖  周世文  汤建林  黄林清 《色谱》2001,19(6):538-540
 建立了测定小鼠血浆、肝、肾、脾、肺等组织中阿昔洛韦 (ACV)浓度的高效液相色谱法。色谱柱为HypersilODS ,流动相为甲醇 水 冰醋酸 (体积比为 1∶99∶0 5 )混合溶液 ,流速为 1 5mL/min ,检测波长为 2 5 2nm。ACV血浆最低检测浓度为 2 0 μg/L ,各组织最低检测浓度为 5 0ng/g。血浆及组织匀浆中的ACV浓度在 0 1mg/L~ 4mg/L及 0 1μg/g~ 4μg/ g时线性关系良好 (r >0 99)。血浆及肝匀浆中的ACV回收率分别为 97 5 %~ 10 0 0 %和 10 0 0 %~ 10 6 0 % (n =5 )。该法精密度高 ,方便 ,快捷 。  相似文献   

6.
秦永平  邹远高  梁茂植  余勤 《分析化学》2004,32(9):1216-1218
采用柱切换技术 荧光检测反相高效液相色谱法测定血浆中特布他林 (TB)浓度。使用LunaC8( 2 )和KromasilC18为分析柱 ( 1 5 0mm× 4.6mm ,5 μm)和预处理柱 ( 2 5mm× 4.6mm ,5 μm) ,流动相分别为pH 3 0 ,0 .0 3 3mol/L磷酸盐缓冲液∶甲醇∶乙腈 ( 92∶7∶1 )和水∶甲醇∶乙腈 ( 97∶2∶1 ) ,流速均为 1 .0ml/L。血浆样品经乙腈沉淀蛋白后进样 ,切换时间为 3 .2~ 4.2min。荧光检测 ,λex为 2 80nm ,λem为 3 0 9nm。以沙丁胺醇作内标 ,按内标法定量。标准曲线线性范围为 0 .8~ 3 2 μg/L ;最低定量限为 0 .8μg/L;TB和内标的保留时间分别为 8.7和 9.3min;日内RSD小于 4% ,日间RSD小于 9% ,方法回收率在 93 %~ 1 1 2 %。  相似文献   

7.
将镀铜镉柱应用于流动注射(FIA)实现了水中硝酸盐氮和亚硝酸盐氮的同时测定。在磷酸介质中,亚硝酸盐与磺胺重氮化,再与N-(1-萘基)-乙二胺盐酸盐偶合,形成玫瑰红色的偶氮染料,在540nm的波长处检测。硝酸盐被镉柱在线还原为亚硝酸盐后同法测定。硝酸盐和亚硝酸盐的测定范围分别为0.1~35mg/L、0~1200μg/L,检出限分别为45.6μg/L和4.8μg/L,RSD均低于1.05%(n=11),测定频率为10样/小时。实际水样中硝酸盐和亚硝酸盐的测定取得了满意的效果,加标回收率均在89.2%~109.0%之间,该仪器适合于现场即时监测。  相似文献   

8.
固相萃取-高效液相色谱法同时测定克伦特罗和沙丁胺醇   总被引:8,自引:0,他引:8  
提出用固相萃取 -高效液相色谱法同时测定饲料中微量克伦特罗和沙丁胺醇的新方法。选用 Dikma Diamonsil C18-ODS分析柱 (2 0 0× 4.6mm,5μm) ,乙腈 -0 .0 1mol/ L KH2 PO4 (p H 3 .0 )作流动相 ,应用波长编程进行检测。克伦特罗和沙丁胺醇的线性范围为 0 .1~ 1 0 0μg/ m L,相关系数分别为 0 .99999和 0 .99977,检出限分别为0 .3 1 ng/ m L和 0 .2 4ng/ m L ,回收率分别为 91 .2 %~ 92 .0 %和 91 .9%~ 93 .0 % ,相对标准偏差分别是 1 .2 0 %~ 2 .0 5%和 1 .2 9%~ 2 .51 %。  相似文献   

9.
反相高效液相色谱法测定3种中成药中的葛根素   总被引:7,自引:0,他引:7  
田菁  黄阁  赵怀清  李发美 《色谱》2001,19(5):457-460
 建立了测定小儿清感灵片、步长新脑心通胶囊和感冒清热颗粒 3种中成药中葛根素含量的反相高效液相色谱方法。采用APEXODS色谱柱 ,以醋酸铵缓冲液 (10 0mmol/L ,pH 5 0 ) 甲醇 (体积比为 75∶2 5 )的混合溶液为流动相 ,检测波长为 2 5 0nm ,流速为 0 8mL/min。葛根素在 2mg/L~ 2 0mg/L时其色谱峰面积与质量浓度的线性关系良好 (r =0 9999) ;上述 3种中成药中的葛根素含量分别为 3 48mg/g ,1 0 8mg/ g及 1 5 2mg/ g(蔗糖型 ) ;其加样回收率分别为 99 0 % ,93 4%和 97 5 %。该法简便、快速、专属性强 ,可以作为多种中药制剂中葛根素含量的测定方法。  相似文献   

10.
气相法分析3-氯-2-羟丙基三甲基氯化铵中的微量有机杂质   总被引:9,自引:0,他引:9  
刘付芳  孙洁  孙惠莲 《色谱》2002,20(4):362-363
 以氯仿为萃取剂 ,对 3 氯 2 羟丙基三甲基氯化铵 (CHPTMA)水溶液进行萃取 ,用气相法分析了CHPT MA溶液中的微量有机杂质环氧氯丙烷和 1 3 二氯丙醇。柱为 2m× 3mmi d 的不锈钢填充柱 ,固定相为10 %的PEG 2 0M ,载体为ChromosorbW/AW。环氧氯丙烷和 1,3 二氯丙醇的回收率分别为 97 5 %~ 10 5 0 %和93 3%~ 98 8% ,相对标准偏差分别为 11 5 %和 13 1% ,最低检测限分别为 5 0 μg/g和 10 0 μg/ g。  相似文献   

11.
A total of 50 commercial samples of Aurantii Fructus, originating from Poncitrus trifoliata for Aurantii Fructus Immaturus, Citrus aurantium, and C. wilsonii for Aurantii Fructus Maturus, respectively, were collected from Taiwan and China herbal markets. Contents of the constituents in the samples were determined within 60 min using a developed HPLC method, which had been validated in terms of precision, repeatability, and accuracy. The results of the analyses showed that the constituents were closely related to the species and also the degree of maturity of the fruits, especially in the case of hesperidin (HE), naringin (NG), neohesperidin (NE), naringenin-7-glucoside (NGC), narirutin (NR), and quercetin (QU). The mature fruits (C. aurantium and C. wilsonii) contained chiefly NG, HE, and NE and the immature ones (P. trifoliata) had NG, NR, and QU majorly. Within the mature samples, the ratios of HE/NE and NGC/NE values were higher than 2.94 and 0.21 in C. aurantium and lower than 1.31 and 0.02 in C. wilsonii, respectively. A flowchart that is useful for identifying Aurantii Fractus was devised, based on the various chemical identification methods.  相似文献   

12.
This study presents an efficient strategy based on microwave‐assisted extraction (MAE), HPLC‐DAD‐MS/MS and high‐speed counter‐current chromatography (HSCCC) for the rapid extraction, identification, separation and purification of active components from the traditional Chinese medicine Fructus Aurantii Immaturus. An LC‐DAD‐MS/MS method was applied for the screening and structural identification of main components in crude extract, and five components were preliminarily identified as neoeriocitrin, narirutin, naringin, hesperidin and neohesperidin according to their UV and mass spectra. An efficient MAE method for the extraction of the three most abundant components (narirutin, naringin and neohesperidin) was optimized by the combination of univariate and multivariate approaches. The crude extract was then separated and purified by HSCCC and a total of 61.6 mg of narirutin, 207.3 mg of naringin and 159.5 mg of neohesperidin at high purities of 98.1, 97.2 and 99.5%, respectively, were obtained from 1.42 g of crude extract. The recoveries of these compounds were 86, 93 and 89%, respectively. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

13.
Twenty commercial samples of Aurantii Fructus Immaturus (Poncitrus trifoliata) and 30 of Aurantii Fructus Maturus (Citrus aurantium and C. wilsonii) were collected from the Taiwan and China herbal markets. The contents of 12 constituents in these samples were determined by HPLC and were used to assess the potential relationships with their plant origins. Multivariate analysis including principal component analysis (PCA), cluster analysis (CA), and linear discriminant analysis (LDA) were used as classification procedures. Natural groupings of the samples divided into three sets successfully, 20 P. trifoliata, 15 C. aurantium, and 15 C. wilsonii, were observed by using PCA and CA. The application of LDA gave correct assignation percentages of 100.0% for all three groups.  相似文献   

14.
The present study aimed to develop a strategy involving quantitative analysis of multicomponents by single marker in combination with high‐performance liquid chromatography fingerprint qualitative analysis for performing the quality control of Aurantii Fructus. The content of 12 components (eriocitrin, neoeriocitrin, narirutin, naringin, hesperidin, neohesperidin, meranzin, poncirin, naringenin, nobiletin, tangeretin, and auraptene) in samples was determined using reliable relative correction factors that were obtained using naringin as an internal reference standard. The new method demonstrated good applicability, and no significant differences were observed between the external standard method and the new method as determined by calculating standard method difference. Qualitative evaluation of samples was conducted using similarity analysis, hierarchical cluster analysis, and quality fluctuation analysis. Chromatographic fingerprint data were divided into three groups by similarity and hierarchical cluster analyses, and seven components may have a more significant impact on the quality of Aurantii Fructus in quality fluctuation analysis. Overall, the study suggests that the qualitative and quantitative analyses of multicomponents using quantitative analysis of multicomponents by single marker combined with chromatographic fingerprinting can be considered good quality criteria for performing quality control and providing technical support for the further pharmacological and pharmaceutical research of Aurantii Fructus.  相似文献   

15.
Investigation of EtOAc fraction from the 95% ethanol extract of Aurantii Fructus Immaturus led to the isolation of one new chromone (1) and seven known flavonoids (28). Their structures were elucidated mainly by NMR and HR-ESI-MS, as well as on comparison with the reported NMR data. The final substituent pattern of 1 was defined by comparison of 13C NMR data calculated by DFT/GIAO with those of experimental NMR data.  相似文献   

16.
In this work, molecularly imprinted solid-phase extraction (MISPE) has been used to selectively enrich, purify, or remove synephrine from Aurantii Fructus Immaturus. To this end, a molecularly imprinted polymer (MIP) was prepared by self-assembly from the template synephrine, the functional monomer methacrylic acid, and the crosslinker ethylene glycol dimethacrylate in 1:4:20 molar ratio. Subsequent molecular interrogation of the MIP binding sites revealed preferential structural selectivity for synephrine relative to other structurally related naturally occurring compounds (i.e. octopamine and tyramine ). This selectivity was subsequently exploited to achieve substantial sample clean-up of extracts of crude Aurantii Fructus Immaturus and Aurantii Fructus Immaturus stir-baked with bran. The purity of synephrine in the extracts after MISPE represented approximately 24.21-fold enrichment of the synephrine in the untreated extracts of Aurantii Fructus Immaturus stir-baked with bran. High recoveries (85–90%) from the samples proved that the method was valid for selective enrichment, purification, or removal of synephrine from Aurantii Fructus Immaturus.  相似文献   

17.
陈锥  陶益  王怡  王毅 《高等学校化学学报》2012,33(12):2692-2696
提出了一种磁珠收集与液相色谱-质谱联用(LC-MS)结合用于快速筛选中药提取物中的脂肪酶抑制剂的方法. 通过制备键合脂肪酶的磁珠, 将其与枳壳总黄酮孵育后, 筛选出枳壳中脂肪酶的配体. 通过LC-MS分析发现, 4个化合物均是潜在的脂肪酶抑制剂, 鉴定其分别为柚皮苷、 新橙皮苷、 橙皮苷和枸橘苷. 对4个化合物进行了体外脂肪酶抑制活性验证. 研究结果表明, 新橙皮苷、 橙皮苷和枸橘苷具有显著的脂肪酶抑制活性, IC50分别为48.04, 52.45和46.18 μg/mL, 其中枸橘苷具有脂肪酶抑制活性为首次报道. 结果表明, 磁珠富集与LC-MS集成技术能够用于快速发现中药活性成分.  相似文献   

18.
张弦飞  杨军丽  陈娟  师彦平 《色谱》2018,36(5):417-424
枸杞作为传统的中药材,具有滋补肝肾、益精明目的功效,亦可作为功能性食品被广泛食用。基于超高效合相色谱-质谱(UPC~2-MS),建立了一种快速、灵敏地定量测定枸杞中甜菜碱(指标化合物)含量的新方法。采用ACQUITY UPC2BEH 2-EP色谱柱(150 mm×2.1 mm,1.7μm),以0.7 mL/min超临界CO_2-甲醇(80∶20,v/v)等度洗脱,成功分离了枸杞中的甜菜碱。在该分离过程中,0.1%(v/v)甲酸作为改性剂;背压为1.31×10~7Pa;柱温为40℃;进样体积为1μL;保留时间为3 min。质谱检测工作于电喷雾(ESI)正离子模式和选择离子监测(SIR)模式。在上述条件下得到线性回归方程。其相关系数为0.999 2,检测范围为0.5~50.0μg/mL,检出限为0.013μg/mL。随后,通过对精度、重复性、稳定性和加标回收率(平均值96.3%)的分析,验证了该方法的有效性。最后,将所建立的方法应用于11批样品的分析。结果表明,该方法可较好地用于枸杞的质量控制与分析评价。  相似文献   

19.
非水反相高效液相色谱法分离测定枸杞子中的类胡萝卜素   总被引:12,自引:0,他引:12  
李忠  彭光华  张声华 《色谱》1998,16(4):341-343
 采用非水反相高效液相色谱法在ODS柱上比较了不同流动相系统对枸杞子中类胡萝卜素的分离效果,探索了枸杞子中类胡萝卜素的最佳分离条件。  相似文献   

20.
构建了一种新的微乳体系,用于微乳液相色潜同时分析吴茱萸药材中的辛弗林、吴茱萸碱和吴茱萸次碱.用甲醇超声提取方法制备样品,通过对表面活性剂种类及浓度、酸度、添加剂等影响因素进行考察,得到最佳微乳体系的组成为:3.0%SDS-6.0%正丁醇-0.6%正辛烷-1.0%甲酸-1.2%乙腈-88.2%水.选择Diamonsil ...  相似文献   

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