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 共查询到19条相似文献,搜索用时 120 毫秒
1.
高效毛细管电泳法测定中草药川乌、草乌中乌头碱的含量   总被引:12,自引:0,他引:12  
孙爱民  陈德华  毕培曦 《色谱》1999,17(1):67-70
 建立了测定有毒中草药川乌和草乌中3种乌头碱的高效毛细管电泳方法,系统地考察了电泳条件对分离的影响,并应用于香港市售川乌及草乌中中乌头碱、次乌头碱和乌头碱的测定。检测限为1.67~2.31mg/L,回收率为93.0%~104.0%,相对标准偏差为0.68%~1.70%。  相似文献   

2.
张盼盼  张福成  王朝虹  蒋晔  卢永江 《色谱》2013,31(3):211-217
建立了超高效液相色谱-串联质谱(UPLC-MS/MS)结合中空纤维微萃取(HF-LPME)同时检测尿样中痕量的乌头碱、次乌头碱、新乌头碱和滇乌头碱等4种生物碱的方法。采用HF-LPME对尿样进行提取、纯化和富集,富集倍数达102~301。同时采用电喷雾电离(ESI)、多反应监测(MRM)进行含量测定,显著提高了尿液中乌头类生物碱的检测灵敏度,4种乌头类生物碱的定量限达到0.01~0.1 ng/L,可大大延长中毒患者尿样中乌头类生物碱的检测时间窗。方法验证结果表明,尿液中乌头碱、新乌头碱和滇乌头碱在0.01~10 ng/L、次乌头碱在0.1~100 ng/L范围内线性关系良好,提取回收率为80.2%~109%,相对标准偏差小于4.6%。该方法适用于乌头类生物碱中毒案件的检测,为痕量乌头类生物碱分析提供了灵敏的分析方法。  相似文献   

3.
陈燕方  何伟  祝凤池 《色谱》2002,20(3):253-255
 选择十八烷基键合相柱 ,以甲醇 水 氯仿 三乙胺 (体积比为 6 8∶32∶2∶0 1)混合溶液为流动相 ,用高效液相法测定了一种植物性农药 0 2 5 %乌头总碱乳油中的乌头生物碱。实验结果表明中乌头碱、乌头碱及次乌头碱与其他杂质能够得到很好的分离。以安宫黄体酮作内标物 ,用峰面积比测定各生物碱含量 ,在其线性范围内分析结果准确 ,回收率高 (>92 % ) ,重现性好 (RSD <3 2 % ) 。  相似文献   

4.
李英和  陈迪华 《化学学报》1994,52(2):204-208
从短距乌头(Aconitum brevicalcaratum Diels)的根中分得六个二萜生物碱成分,其中三个为新成分,即短距乌碱甲(acobretine A,1),短距乌碱乙(acobretine B,2)和短距乌碱丙(acobretine C,3).另三个为已知成分:花葶乌头宁(scaconine,4),花葶乌头碱(scaconitine,5)和N-脱乙酰花葶乌头碱(N-deacetylscaconitine,6).经IR,MS,^1H NMR,^1^3C NMR测定和化学方法确定可1~3的结构  相似文献   

5.
王朝虹  叶敏  邢俊波  何毅  果德安 《色谱》2005,23(3):316-316
为配合乌头类药材合理应用,本文建立了高效液相色谱-质谱联用(HPLC—MS)测定组织样品中乌头碱的方法,并对急性中毒大鼠体内的乌头碱分布进行了测定。  相似文献   

6.
反相胶束增稳荧光法测定兔血浆中痕量盐酸水檗碱的研究   总被引:1,自引:0,他引:1  
本文研究了气溶胶(AOT)/环已烷/水反相胶束介质中中草药有效成分盐酸小檗碱的荧光性质,并将该法应用于兔血浆中痕量盐酸小壁碱的测定。该法的线性范围为1.0×10-7~3×10^-5(g/ml),检出限为8.3×10^-8(g/ml),相对标准偏差为1.1%。  相似文献   

7.
反相胶束增稳荧光法测定兔血浆中痕量盐酸小檗碱的研究   总被引:2,自引:0,他引:2  
本文研究了气溶胶(AOT)/环己烷/水反相胶束介质中中草药有效成分盐酸小檗碱的荧光性质,并将该法应用于兔血浆中痕量盐酸小檗碱的测定。该法的线性范围为1.0×10- 7~3×10- 5(g/m L),检出限为8.3×10- 8(g/m L),相对标准偏差为1.1% 。  相似文献   

8.
高效液相色谱法测定血浆中莲心碱的浓度   总被引:1,自引:0,他引:1  
张先洲  文为  胡学民  罗顺德  蔡鸿生 《色谱》1997,15(4):347-348
 采用高效液相色谱法(甲基莲心碱为内标)测定了血浆中莲心碱的浓度。以UltrasphereSi为固定相、二氯甲烷-异丙醇-二乙胺(75150.2,V/V)为流动相,检测波长为282nm。血样用氨-氯化铵缓冲液调pH10后用乙醚提取。平均回收率93.6%,RSD为1.9%,最低检测浓度0.025mg/L。  相似文献   

9.
于科岐  董社英  李华  高鸿 《分析化学》1999,27(9):1003-1006
提出微机化的干净人微分示波计时电位法。在B-R缓冲液(PH2)中,希夫碱在dE/dt-E示波图上产生灵敏的切口,切口电位E=-0.91V;在1.80×10^-5 ̄1.14×10^-4mol/L范围希夫碱的浓度与二次微分曲线上去极剂峰高呈线怀关系,r=0.9966;RSD≤6.0%,合成样品测定回收率在97.9-102.5%。  相似文献   

10.
Liu M  Zhang S  Yang C  Xia Y  Liu J  Liang J 《色谱》2011,29(5):430-434
应用高速逆流色谱法分离制备了生附子中的3个C19型二萜生物碱类化合物。以正己烷-乙酸乙酯-甲醇-水(3:5:4:5, v/v/v/v)为两相溶剂系统,上相为固定相,下相为流动相,在主机转速850 r/min、流动相流速2.0 mL/min、检测波长235 nm条件下进行分离制备;一次性从90 mg附子总碱粗提物中分离制备得到15.3 mg北草乌碱,35.1 mg中乌头碱和22.7 mg次乌头碱,经高效液相色谱分析,测得它们的纯度分别为97.9%、96.2%和99.2%。并应用波谱(电喷雾离子质谱、核磁共振氢谱和核磁共振13C谱)解析法确定了它们的结构。利用该方法可以对生附子中的二萜类生物碱成分进行快速的分离和纯化  相似文献   

11.
The determination of three aconitine alkaloids (hypaconitine, aconitine, mesaconitine) in five traditional Chinese medicines including two Tibetan medicines, Chuanwu, Caowu, Fuzi, Aconitum Tanguticum Maxim and Aconitum Gymnandrum Maxim by non-aqueous capillary electrophoresis using a new recording mode is described. The dissociation constants of aconitine, mesaconitine and hypaconitine have also been determined by CZE and were 7.71, 6.60 and 6.25, respectively. The separation was achieved by optimizing the applied voltage, the pH and the concentration of the buffer. The electrophoretic medium was 20 mM borax-70% (v/v) methanol (pH 8.5) and an uncoated capillary (50 cm x 75 microm i.d.) was used. Detection was carried out with a UV monitor at 214 nm. The total time for separation and determination was under 13 min.  相似文献   

12.
An electrospray ionization / tandem mass spectrometric (ESUMS/MS) method was developed for the simultaneous identification and analysis of three aconitine alkaloids [mesacontine (MA), hypaconitine (HA), and aconitine (A)] as intact molecules at low nanogram level in Chinese traditional medicine Chuanwu decoction as well as in human whole blood extract without chromatographic separation.  相似文献   

13.
Bao Y  Yang F  Yang X 《Electrophoresis》2011,32(12):1515-1521
A CE‐electrochemiluminescence(CE‐ECL) detection system, CE/tris(2,2′‐bipyridyl) ruthenium(II)ECL with ionic liquid, was established for the determination of diester‐diterpenoid aconitum alkaloids (aconitine (AC), mesaconitine (MA) and hypaconitine (HA)) in traditional Chinese herbal medicine. Running buffer containing 25 mM borax‐20 mM 1‐ethyl‐3‐methylimidazolium tetrafluoroborate at pH 9.15 was used, which resulted in significant changes in separation and obvious enhancement in ECL intensity for AC, MA and HA with similar structures. End‐column detection was achieved in 50 mM phosphate buffer with 5 mM (pH 9.15) at applied detection voltage of 1.20 V when the distance between the Pt working electrode and outlet of capillary (50 cm×25 μm id) was set at 150 μm. One single quantitative analysis of three alkaloids was achieved at a separation voltage of 15 kV within 10 min. Moreover, two extraction processes (ethanol extraction and ethyl ether extraction after basification) were investigated. The result showed that ethanol extraction process has higher extraction efficiency than ethyl ether extraction process. Under the optimized conditions, the detection limits of AC, MA and HA were 5.62×10?8, 2.78×10?8 and 3.50×10?9 mol/L (S/N=3), respectively. The method was successfully applied to determine the amounts of AC, MA and HA in the aconitum herbal samples.  相似文献   

14.
Yin J  Guo W  Du Y  Wang E 《Electrophoresis》2006,27(23):4836-4841
A facile CE method coupled with tris(2,2'-bipyridyl) ruthenium(II)-based electrochemiluminescence [Ru(bpy)(3) (2+)] detection was developed for simultaneous determination of Aconitum alkaloids, i.e., hypaconitine (HA), aconitine (AC), and mesaconitine (MA) in baseline separation. The optimal separation of these Aconitum alkaloids was achieved in a fused-silica capillary column (50 cm x 25 microm id) with 30 mM phosphate solution (pH 8.40) as running buffer at 12 kV applied voltage. The three alkaloids can be determined within 10 min by a single run. The calibration curves showed a linear range from 2.0 x 10(-7) to 2.0 x 10(-5) M for HA, 3.4 x 10(-7) to 1.7 x 10(-5) M for AC, and 3.8 x 10(-7) to 1.9 x 10(-5) M for MA. The RSDs for all analytes were below 3.01%. Good linear relationships were found with correlation coefficients for all analytes exceeding 0.993. The detection limits were 2.0 x 10(-8) M for HA, 1.7 x 10(-7) M for AC, and 1.9 x 10(-7) M for MA under optimal conditions. This method was successfully applied to determine the three alkaloids in Aconitum plants.  相似文献   

15.
Li Y  Qi S  Chen X  Hu Z 《Electrophoresis》2004,25(17):3003-3009
An easy, rapid, and simple nonaqueous capillary electrophoresis (NACE) method was developed for the identification and determination of three aconitine alkaloids, hypaconitine (HN), aconitine (AN), and mesaconitine (MN) within 6 min. The most suitable running buffer was composed of 60 mM ammonium acetate, 0.5% acetic acid, and 15% acetonitrile (ACN) in methanol with a fused-silica capillary column (50 cm x 75 microm ID). In the concentration range 12.5-1000 mg/L the calibration curves reveal linear relationships between the peak area for each analyte and its concentration (correlation coefficients: 0.9997 for HN, 0.9999 for AN, and 0.9995 for MN). The relative standard deviations of the migration time and peak area of the three alkaloids were 0.13, 0.57, 0.33 and 2.87, 1.06, 3.49%, respectively. The method was successfully applied to determine the three alkaloids in two commonly used traditional Chinese herbal medicines, the recoveries of the three constituents ranging between 94.7-101.9% for HN, 98.3-102.3% for AN, and 98.1-104.6% for MN.  相似文献   

16.
建立了电堆积在线扫集胶束电动色谱法测定苦参碱和槐定碱的新方法.考察了pH值、磷酸二氢钠浓度、CTAB浓度、电压、有机溶剂和进样时间对分离效果的影响.采用未涂层熔融石英毛细管,以20mmol/L磷酸二氢钠-0.8 mmol/L CTAB-100mmol/L Tris(含10%异丙醇,pH 8.9)为缓冲液,在进样电压-1...  相似文献   

17.
Large‐volume sample stacking (LVSS) is commonly used as an effective online preconcentration method in capillary zone electrophoresis (CZE). In this paper, the method LVSS combined with CZE has been proposed to analyze camptothecin alkaloids. Optimum separation can be achieved in the following conditions: pH 9.0; 25mm borate buffer containing 20 mm sulfobutylether‐β‐cyclodextrin and 20 mm ionic liquid 1‐ethyl‐3‐methyllimidazole l ‐lactate; applied voltage 20 kV; and capillary temperature 25 °C. The LVSS was optimized as hydrodynamic injection 4 s at 5.0 psi and the polarity switching time was 0.17 min. Under the above conditions, the analytes could be separated completely in <20 min and the detector response was increased compared with conventional hydrodynamic injection. The limits of detection were between 0.20 and 0.78 μg/L. A good linearity was obtained with correlation coefficients from 0.9991 to 0.9997. The recoveries ranged from 97.72 to 103.2% and the results demonstrated excellent accuracy. In terms of the migration time and peak area, the experiment was reproducible. The experimental results indicated that baseline separation can be obtained and this method is suitable for the quantitative determination of camptothecin alkaloids in real samples.  相似文献   

18.
毛细管电泳-激光诱导荧光检测法测定抗癫痫药加巴喷丁   总被引:1,自引:0,他引:1  
蔡元丽  杨甲甲  王宇飞  白珂珂  李晖 《色谱》2010,28(12):1179-1184
建立了毛细管电泳-激光诱导荧光(CE-LIF)测定抗癫痫药加巴喷丁的方法。加巴喷丁经4-氯-7-硝基苯并-2-氧杂-1,3-二唑(NBD-Cl)衍生化后,采用10mmol/L硼砂-10mmol/L十二烷基硫酸钠(pH9.75)的缓冲体系,加巴喷丁在6min内实现高效基线分离。方法的线性范围为0.01~10mg/L(r=0.999 7),检出限为2μg/L,定量限为10μg/L。方法的平均回收率为100.2%~103.1%,相对标准偏差为0.15%~1.00%(n=3)。该方法灵敏、快速、准确和可靠,已用于加巴喷丁药物制剂的质量控制。  相似文献   

19.
建立了高效毛细管电泳-电喷雾飞行时间质谱联用(HPCE-ESI-TOF/MS)快速定性分析黄连中生物碱类化合物的分析方法. 使用未涂层石英毛细管, 以50 mmol/L乙酸铵-0.5%甲醇溶液(用氨水调至pH=7.2)作为运行缓冲液, 分离电压为25 kV; 鞘液组成为50%甲醇-49.5%水-0.5%乙酸, 鞘液流速为4 μL/min; 质谱选用正离子模式, 碰撞电压(Fragmentor)为100 V. 结果表明, 通过各色谱峰紫外光谱和质谱测得精确分子量结果, 结合文献, 对黄连中7种生物碱进行了鉴定. 表明本方法简便、快速, 是黄连中生物碱类化合物快速分离、鉴别的有效方法.  相似文献   

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