HPLC法同时测定双黄连制剂中绿原酸、黄芩苷和连翘苷的含量

目的：建立以HPLC法同时测定双黄连制剂中三种指标成分含量的方法。方法：采用Amethyst C18-P色谱柱,流动相为乙腈-0.4%磷酸,流速为1.0ml/min,检测波长为230nm,柱温为30℃。结果：绿原酸在7.52～150.40μg/ml、黄芩苷在4.98～99.60μg/ml、连翘苷在0.76～15.20μg./ml浓度范围内,三种指标成分线性关系良好,RSD均大于0.9988;三种指标成分的加样回收率分别为96.75%（RSD=1.28%）,99.58%（RSD=1.60%）,和104.48%（RSD=2.96%）。结论：本方法简便、结果准确可靠,可有效控制双黄连制剂的质量。     

HPLC测定双黄连口服液中连翘苷的含量实例

目的验证双黄连口服液中连翘苷的测定方法。方法采用HPI。C法测定双黄连口服液中连翘苷的含量。结果分别连续进样（10．0μl）5次,测得连翘苷色谱峰峰面积336756,336672,337035,336062,336750,平均值336655、RSD0．1％。结论所建立的方法简便、准确、可靠,可作为双黄连口服液的质量控制方法。     

HPLC法测定注射用双黄连中黄芩苷、野黄芩苷、黄芩素、〖JZ〗咖啡酸和绿原酸

目的 建立同时测定注射用双黄连中黄芩苷、野黄芩苷、黄芩素、咖啡酸和绿原酸5种有效成分的方法。方法 高效液相色谱法。Phenomenex C₁₈色谱柱(250 mm×4.6 mm,5 μm);流动相：乙腈-1%冰醋酸水溶液,作梯度洗脱;检测波长为327 nm;体积流量为1 mL/min;柱温为40 ℃,灵敏度为0.100 0 AUFS。结果 在筛选色谱条件下,测定了注射用双黄连中的黄芩苷、野黄芩苷、黄芩素、咖啡酸和绿原酸5种有效成分。结论 本方法简便、快速、准确、可靠,可用于注射用双黄连中有效成分的测定。     

黄芩苷的体内药代动力学研究进展

黄芩为唇形科多年生草本植物黄芩 (Scuellaria baicalens-is Georgi)的根 ,主要含黄芩苷 (baicalin)、黄芩素 (baicalein)等多种黄酮类化合物。黄芩能清热燥湿、泻火解毒、止血、安胎 ,用于肺热咳嗽 ,高热烦渴、血热吐血、衄血 ,泻痢、黄疸、胎动不安、痈肿疮毒、高血压头痛 ,近来研究发现其具有抗氧化、抗癌防癌、抗菌、抗病毒、增强免疫等作用 [1 ] 。黄芩苷是黄芩的主要有效成分之一 ,是黄芩及其制剂的主要质量控制指标 ,本文就其在体内的药代动力学研究进展综述如下。1　研究对象　　动物试验以普通 Wistar、SD大鼠、健康家兔 [2～ 4 …     

连翘提取物和连翘酯苷A原料中连翘酯苷A的稳定性研究

目的 考察连翘提取物及其主要有效成分连翘酯苷A的稳定性,为更好控制连翘提取物质量提供依据。 方法 采用高温、高湿、强光照射等影响因素试验及加速试验对样品在固体状态下以及水溶液中的稳定性进行系统研究。 结果 固态条件下湿度对连翘酯苷A稳定性影响较大,光照次之,温度影响不大;在水溶液中,酸性条件及抗氧剂的加入能改善其稳定性,维生素C(Vc)能显著提高其在溶液中的稳定性。 结论 固态条件下,要保持连翘提取物及连翘酯苷A稳定,须对湿度、光照加以控制;水溶液中,酸性介质及抗氧剂的加入有利于改善水溶液中连翘酯苷A的稳定性。     

黄芩苷灌胃后在兔眼晶状体中的药代动力学研究

目的通过黄芩苷灌胃后,根据各组日本大耳白兔晶状体中黄芩苷浓度的变化,研究黄芩苷在晶状体中的药代动力学特点.方法 44只日本大耳白兔随机分成11组,各组每只白兔按80 mg/kg黄芩苷灌胃,在用药前(0h)和用药后0.25,0.50,0.75,1,1.5,2,3,5,8,12h取晶状体,采用反向高效液相色谱法进行测定.结果黄芩苷浓度在15min时为(1.069±0.153)μg/ml,0.5h时达高峰,峰值为(4.765±0.876)μg/ml,在0.5～0.75h内迅速下降,0.75～1.5h之间缓慢下降,降至(1.611±0.485)μg/ml后又有所升高,至2h时达第二个峰值(2.975±0.875)μg/ml,随后逐渐下降,5h降至(0.862±0.328)μg/ml,8、12h晶状体中黄芩苷的浓度很微量,基本测不到.结论本方法灵敏、特异、准确,可用于眼晶状体中黄芩苷浓度的测定;黄芩苷灌胃后能够通过血-眼屏障进入晶状体,这为黄芩苷全身用药治疗眼部疾病提供了实验依据.     

黄芩苷灌胃后在兔眼玻璃体中的药代动力学研究

目的黄芩苷灌胃后不同时间日本大耳白家兔玻璃体中质量浓度变化,研究药代动力学特点。方法44只日本大耳白家兔随机分成11组,各组每只白兔按80 mg/kg黄芩苷灌胃,在用药前(0 h)和用药后0.25,0.50,0.75,1,1.5,2,3,5,8,12 h取玻璃体,采用反向高效液相色谱法进行测定。结果0.25~0.75 h浓度缓慢升高,灌胃后0.75~1 h迅速达高峰,峰值为(0.754±0.093)μg/mL,之后开始下降,3 h降至(0.077±0.002)μg/mL,5~12 h玻璃体中黄芩苷的质量浓度很微量,基本测不到。结论本方法灵敏、特异、准确,可用于眼玻璃体中黄芩苷质量浓度的测定:黄芩苷灌胃后能够通过血-眼屏障进入玻璃体,这一结果为黄芩苷全身用药治疗眼部疾病提供了实验依据。     

RP-HPLC法对复方桑菊清热口服液中绿原酸、蒙花苷、连翘苷的含量测定

目的:建立复方桑菊清热口服中绿原酸、蒙花苷、连翘苷的含量测定方法。方法:采用高效液相色谱法,以乙腈-0.2%醋酸水溶液为流动相梯度洗脱,色谱柱为Agilent C18(250mm×4.6mm,5um),柱温:25℃,检测波长为220nm,流速为1.0ml/min,进样量20μL。结果:绿原酸、蒙花苷和连翘苷的回收率分别为97.82%、97.75%、96.63%;RSD为1.33%、2.67%和1.1%。结论:所用测定方法简单可行,可用于复方桑菊清热口服液质量的质量控制。     

RP-HPLC 法同时测定抗病毒口服液中绿原酸和连翘苷的含量

目的:建立同时测定抗病毒口服液中绿殿酸和连翘苷的反相高效液相色谱方法.方法:采用岛津 Shim-pack VP-ODS 柱(4.6mm×150mm,5μm),流动相为乙腈(A 相),0.02%醋酸(B 相),0～20min 流动相 A 的比例从 5% 线性增加至 25%;流速为 1mL/mim,检测波长为280nm.结果:绿原酸和连翘苷均能良好分离,绿原酸在 2.32～11.60μg/mL 范围内线性关系良好,连翘许在 5～25μg/mL 范围内线性关系良好,分别为 97,89% 和 99,89%.结论:采用 RP-HPLC法对抗病毒口服液进行质量控制,方法简便、标准、重现性好,能排除其它成分的干扰,可用于该制剂的质量控制.     

An LC-MS/MS Method for the Simultaneous Determination of Lycorine and Galanthamine in Rat Plasma and Its Application to Pharmacokinetic Study of Lycoris Radiata Extract in Rats

A rapid, sensitive, and selective liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of lycorine and galanthamine, two major constituents in Lycoris radiata extract, in rat plasma. Liquid-liquid extraction with ethyl ether was carried out using diphenhydramine as the internal standard The two bioactive alkaloids were separated on a Zorbax SB-C18 reserved-phase column （150 mm× 4.6 mm, i.d., 5 μm） by gradient elution using a mobile phase consisting of methanol with 0.1% formic acid （A） and water with 0.1% formic acid （B） at a flow rate of 0.6 mL/min. All analytes showed good linearity over a wide concentration range （r^2〉0.99） and the lower limit of quantification was 3.00 ng/mL for each analyte. The average extraction re- covery of the analytes from rat plasma was more than 82.15%, and the intra-day and inter-day accuracy and preci- sion of the assay were less than 12.6%. The validated method was successfully applied to monitoring the concen- trations and pharmacokinetic studies of two Amaryllidaceous alkaloids in rat plasma after an oral administration of Lycoris radiata extract.     

UPLC法测定银翘解毒口服液中牛蒡苷、蒙花苷、绿原酸、隐绿原酸

目的采用UPLC测定银翘解毒口服液中牛蒡苷、蒙花苷、绿原酸、隐绿原酸。方法色谱柱:C18(2.1mm×100mm,1.7μm),流动相:乙腈-0.1%甲酸水进行梯度洗脱,检测波长300nm,流速0.3mL/min,柱温40℃。结果所检测的各色谱峰分离度良好,方法学实验结果符合UPLC法测定要求。结论该方法可用于银翘解毒口服液的质量控制。     

Simultaneous Determination of Silybin A and Silybin B in Rat Plasma and Pharmacokinetic Study

Objective To investigate the bioavailability and pharmacokinetics of silybin A and silybin B in rats, respectively. Methods Following iv and ig administration of silybin to 20 Wistar rats, the plasma samples were collected at different time points up to 12 h. Sample pretreatment was involved in one-step protein precipitation with acetonitrile. Silybin A and silybin B were simultaneously determined by LC-MS/MS. Results After ig dosing silybin 28, 56, and 112 mg/kg to rats, the t1/2β values were 5.48, 5.08, and 5.73 h for silybin A, and 4.56, 4.12, and 5.53 h for silybin B; The Cmax were 674.3, 1349.4, and 2042.5 ng/mL for silybin A, and 671.0, 1365.4, and 2066.2 ng/mL for silybin B; The Tmax were 0.20, 0.23, and 0.20 h for silybin A, and 0.20, 0.23, and 0.20 h for silybin B; The AUC were 454.4, 845.9, and 1219.5 h?ng/mL for silybin A, and 432.0, 817.1, and 1153.6 h?ng/mL for silybin B. The absolute bioavailabilities of silybin A and silybin B were 2.86% and 1.93%, respectively. Conclusion Silybin A and silybin B have very low bioavailability after ig administration, and there is no significant difference in the pharmacokinetic parameters between silybin A and silybin B, which indicates that the two diastereoisomers have similar pharmacokinetic behavior in rats.     

Determination of Shionone in Rat Plasma by HPLC and its Pharmacokinetic study

Objective To develop a sensitive, simple, and accurate method for the determination of shionone in rat plasma after ig administration of Asteris Radix petroleum ether extract (RAPE). Methods The separation was achieved by HPLC on a RP18 column (150 mm × 3.9 mm, 5 μm) with a mobile phase composed of acetonitrile-0.05% phosphoric acid water (98︰2) at a flow rate of 1.0 mL/min. UV Detector was set at 200 nm and friedelin was chosen as an internal standard. Results The linear range of the standard curves was (0.3443–22.0) μg/mL with the correlation coefficient of 0.9968. The intra- and inter-day precisions were all below 10% and the relative error was ?3.5%–1.1%. Conclusion The developed method can be successfully applied to the pharmacokinetic study. After ig administration of RAPE, T1/2(ka) is (33.09 ± 7.32) min and T1/2(ke) is (84.95 ± 22.34) min.     

A Specific and Sensitive LC-MS/MS Method for Simultaneous Determination of Four Major Active Catechins of Tea Polyphenols in Rat Plasma and Its Application to Pharmacokinetic Study

Objective To develop a liquid chromatography technique coupled with tandem mass spectrometry (LC-MS/MS) for simultaneous determination of four active catechins EGCG, ECG, EGC, and EC of tea polyphenols (TP) in rat plasma in order to further study its multi-component pharmacokinetics. Methods Following a single step liquid-liquid extraction of plasma samples with ethyl acetate, the four catechins were separated on a Hypersil ODS C18 column using an isocratic mobile phase composed of methanol-water (30︰70). The detection using a mass spectrometer was performed under negative ESI in the MRM mode. The analytes were identified by reference to both MRM and tR values and quantified using peak area internal standard method. Results The method was shown to be specific without interference from matrix, metabolites, and impurities present in TP raw material and to be sensitive with LOD and LOQ of 1.5 and 10 ng/mL (EGCG) as well as 0.75 and 5 ng/mL (ECG, EGC, and EC). A good linearity was obtained over a wide range of 10-10 000 ng/mL for EGCG and 5-5000 ng/mL for other three catechins (r > 0.996). The method was validated to be reproducible and reliable, as evidenced by intra-batch and inter-batch precision of less than 10% and 11%, accuracy of 97.13%-106.05% and 99.22%-103.14%, respectively. The recovery of extraction ranged from 72.74% to 89.13%, matrix effect from 88.76% to 105.97% for four catechins. The method was successfully used to study the pharmacokinetics of TP iv administered to rats at a dose of 100 mg/kg. Conclusion This method is shown to completely meet requirements for the multi-component pharmacokinetic study of TP in rats.     

栀子药材中栀子苷和绿原酸含量测定方法研究

目的：建立栀子药材中栀子苷和绿原酸含量测定方法。方法：色谱柱为DiamonsilC18柱（250mm×4．6mm,5μm）;流动相为1．0％的冰乙酸水溶液-1．0％冰乙酸乙腈溶液梯度洗脱;检测波长为238nm;流速1．0mL／min;柱温30℃;进样量10μL。结果：栀子苷在3171-12685μg／mL质量浓度范围内线性关系良好,r=0．9999（n=6）,平均回收率为99．98％,IKSD为0．33％;绿原酸在1．952-78．08μg／mL质量浓度范围内线性关系良好,r=0．9999（n=6）,平均回收率为100．6％,1KSD为0．81％。结论：方法操作简便,结果准确,可用于栀子药材中的栀子苷、绿原酸含量测定。     

绿原酸提取及分析测定方法研究进展

绿原酸为金银花的主要抗菌有效成分,它具有抗菌、抗病毒、解热、升高白细胞、保肝利胆、免疫调节、抗肿瘤、降血压、降血脂、清除自由基等作用.将绿原酸的提取及分析测定方法的研究近况综述.     

清热养心颗粒的鉴别及其绿原酸含量测定

目的:建立清热养心颗粒的质量标准.方法:采用薄层色谱法对6味组方药材进行鉴别,并用HPLC法对组方药材金银花所含绿原酸进行含量测定,Supelco ODS-C18柱(4.6×250mm,5μm),柱温30℃,流动相为乙腈-0.2%磷酸水(8:92),检测波长327nm.结果:金银花、黄连、黄精、百合、山豆根、甘草6昧组方药材经薄层色谱被全部鉴识,各主斑点分离清晰,阴性无干扰;绿原酸对照品在0.01884μg～0.6008μg范围内与色谱峰面积呈良好的线性关系(r=0.9999),加样回收率平均98.5%(n=6,KSD=0.8%).结论:上述定性及定量可用于清热养心颗粒质量控制.     

兔血浆利福平的反相高效液相色谱分析及药代动力学研究

目的建立兔血浆利福平（rifampicin,RFP）反相高效液相色谱分析方法（reversed-phase high-performance liquid chromatography,RP-HPLC）。研究其静脉给药后兔体内血浆药代动力学参数。方法以Agilent ZORBAX XDB-C18柱（5μm,4.6mm×150mm）为分析柱,流动相为0.02mol·L^-1磷酸二氢钠缓冲液（PH7.0）∶甲醇=30∶70;流速1.0mL·min^-1;柱温：35℃,检测波长330nm。8只新西兰大白兔分别按RFP12mg·kg^-1静滴,RP-HPLC法检测血浆药物浓度。所得血药浓度数据经DAS软件拟合分析。结果 RFP在0.5～72μg·mL^-1血浆浓度范围内线性关系良好（r=0.99969）,平均提取回收率为99.72%,日内、日间变异系数（RSD=5）分别为2.6%～4.4%和2.2%～2.9%。静脉滴注RFP在兔体内药代动力学过程符合双隔室模型（权重系数为1/cc）,T1/2=（2.87±0.78）h,Cmax=（12.49±1.57）mg·L^-1,AUC（0-∞）=（50.05±14.50）mg·（h·L）^-1。结论本研究建立的兔血浆利福平RP-HPLC方法简便、准确、重现性好,可用于兔体内利福平血药浓度的测定,兔体内利福平药代动力学过程符合双隔室模型,体内药代谢动力学参数为利福平其它剂型的研究提供参考。     

褶合曲线分析法测定银黄含片中绿原酸和黄芩苷的含量

目的:测定银黄含片中绿原酸和黄芩苷的含量。方法:应用计算机辅助褶合曲线分析法,同时测定绿原酸和黄芩苷的含量。结果:绿原酸和黄芩苷的回收率和相对标准差分别为97.28%、0.88%;98.11%、0.45%。结论:用褶合曲线分析法检测银黄含片中绿原酸和黄芩苷的含量简便、快速,结果可靠。