高效液相色谱法测定清热利胆合剂中黄芩苷的含量

目的研究清热利胆合剂中黄芩苷的定量分析方法.方法采用高效液相色谱法.色谱柱KYWG-C18(4.6mm×150 mm,5μm)分析柱;流动相甲醇-水-磷酸(45550.2,v/v),流速1.0mL·min-1;测定波长278 nm;柱温室温.结果黄芩苷在0.199 2～0.996 0μg(r=0.999 6)呈良好的线性关系,平均回收率为98.34%,RSD为1.18%.结论本法简便、灵敏、准确,可用于清热利胆合剂的质量控制.     

HPLC法测定利胆排石片中黄芩苷的含量

目的建立高效液相色谱法测定利胆排石片中黄芩苷的含量。方法采用色谱柱为Chromanalysis ODS柱(4.6mm×250mm,5μm);流动相为甲醇-水-冰醋酸(48∶52∶1);检测波长278nm;柱温20℃;流速1.0mL/min。结果黄芩苷在2.55~20.4μg/mL的浓度范围内,浓度对峰面积具有良好的线性关系。黄芩苷平均回收率为100.1%,RSD为1.47%。结论建立的HPLC法操作简便、灵敏度高、精密度好,可为利胆排石片的质量控制提供依据。     

RP-HPLC法测定兔血浆中黄芩苷含量

目的采用RP HPLC法测定家兔血浆中黄芩苷的浓度。方法用乙腈沉淀血浆蛋白 ,上清液直接进样测定。色谱柱为DiamonsilTMC18柱 ;流动相为甲醇 水 磷酸 ( 5 0∶5 0∶0 2 ,V∶V∶V) ,流速1 0mL/min ;检测波长为 2 77nm ,以对硝基苯甲酸为内标物。结果在黄芩苷浓度为 0 1～5 0mg/L内线性关系良好 (r =0 9975 ,日内、日间RSD分别≤ 5 4 %和≤ 7 2 % ,平均回收率为1 0 0 1 %。结论方法简便快速 ,适用于黄芩苷的血药浓度测定及药代动力学研究。     

UPLC-MS/MS法测定大鼠血浆中黄芩苷的浓度

目的建立UPLC-MS/MS法测定大鼠血浆中黄芩苷的浓度,并初步研究大鼠尾静脉注射黄芩苷纳米结晶后药动学特征。方法采用液液萃取法提取药物,以地西泮为内标,色谱柱为C8柱(100 mm×2.0mm,2.2μm),0.2%甲酸水溶液-甲醇为流动相,流速为0.4 mL·min-1。样品在三级四极杆串联质谱中经ESI源离子化后以多反应离子监测方式测定。结果黄芩苷的线性范围为5⁵ 000 ng·mL-1,定量下限为5 ng·mL-1,平均方法回收率在87.4%5 000 ng·mL-1,定量下限为5 ng·mL-1,平均方法回收率在87.4%¹00.9%,日内、日间变异系数均<15%。结论方法灵敏、准确、快速、专属性强,适用于黄芩苷的血药浓度测定和药物代谢动力学研究。     

HPLC法同时测定小儿热速清颗粒中绿原酸和黄芩苷的含量

目的:建立同时测定小儿热速清颗粒中绿原酸和黄芩苷含量的方法。方法:采用反相高效液相色谱法。色谱柱为Di-amonsilTM-C18柱,流动相为甲醇-水-磷酸(v/v=52:48:0.1),流速为1mL.min-1,检测波长为323nm,进样量为10μL,柱温为30℃。结果:绿原酸浓度在1.50～40.00μg.mL-1范围内与峰面积积分值呈良好的线性关系,平均回收率为99.22%,RSD=1.45%(n=5)。黄芩苷浓度在0.50～100.00μg.mL-1范围内与峰面积积分值呈良好的线性关系,平均回收率为99.68%,RSD=0.84%(n=5)。结论:本方法灵敏、准确、重复性好,可用于小儿热速清颗粒的质量控制。     

RP-HPLC法测定牛黄上清胶囊中黄芩苷的含量

目的:探讨RP-HPLC法测定牛黄上清胶囊中黄芩苷的含量.方法:采用十八烷基硅烷键合硅胶柱;流动相:甲醇-水-磷酸(47:53:0.2)为流动相,检测波长280nm;流速为1.0 ml/min.结果:黄芩苷线性范围19.935～99.674μg/mL.平均回收率为98.79%,RSD=1.21%.结论:方法简便、快速、结果准确、重现性好,可用于牛黄上清胶囊中黄芩苷的含量测定.     

高效液相色谱法测定双黄口服液中芍药苷和黄芩苷含量

目的建立测定双黄口服液中芍药苷和黄芩苷含量的高效液相色谱法。方法色谱柱为Ultimate XB-C18柱（250mm×4.6mm,5μm）,流动相为甲醇-水-醋酸（35：65：1）,流速1.0mL/min,检测波长244nm。结果芍药苷和黄芩苷质量浓度均在25～250μg/mL范围内与峰面积线性关系良好,相关系数分别为0.9997和1.0000,平均回收率分别为97.74%和97.06%（n=6）。结论所用方法可同时测定双黄口服液中芍药苷和黄芩苷的含量,且方法简便、准确。     

高效液相色谱法测定小儿热速清糖浆中黄芩苷含量

目的建立测定小儿热速清糖浆中黄芩苷含量的高效液相色谱法。方法采用Agilent Extend C18柱(250 mm×4.6 mm,5μm),以甲醇-水-磷酸(47∶53∶0.2)为流动相,流速为0.9 mL/min,检测波长为276 nm,柱温为30℃。结果黄芩苷质量浓度在5.245～78.68μg/mL范围内与峰面积呈良好线性关系(r=1.000 0,n=7),平均回收率为98.74%,RSD为0.59%(n=9)。结论该方法简便、准确,重复性好,可用于小儿热速清糖浆中黄芩苷的含量测定。     

胃必欢颗粒中黄芩苷、盐酸小檗碱含量的测定

目的建立测定胃必欢颗粒中黄芩苷、盐酸小檗碱含量的方法.方法采用高效液相色谱法.色谱柱为BDSC18,流动相为甲醇-水-冰醋酸-三乙胺(33∶61∶6∶0.2,v/v);,流速为1.0 mL·min-1,检测波长为270 nm.结果黄芩苷在16.38～409.50 mg·L-1范围内峰面积与其质量浓度呈良好线性关系,平均回收率为100.2%,(RSD为1.5%);盐酸小檗碱在5.99～149.80 mg·L-1范围内峰面积与其质量浓度呈良好线性关系,平均回收率为102.3%,(RSD为1.3%).结论此法简便、快速、准确,可作为胃必欢颗粒含量测定的方法.     

高效液相色谱法同时测定双黄消炎片中黄芩苷和黄芩素含量

目的 建立同时测定双黄消炎片中黄芩苷和黄芩素含量的反相高效液相色谱法.方法 色谱柱采用Agilent Eclipse XDB-C18柱(250 mm ×4.6 mm,5μm),以甲醇-0.1%磷酸溶液为流动相(梯度洗脱),检测波长为277 nm,流速1.0 mL/min,进样量10μL,柱温35℃.结果 黄芩苷质量浓度在5.678~141.95μg/mL范围内与峰面积有良好线性关系,r=1.000 0(n=7);黄芩素质量浓度在2.122~53.05 μg/mL范围内与峰面积有良好线性关系,r=1.000 0(n=7).黄芩苷平均回收率为99.32%,RSD为0.63%(n=6);黄芩素平均回收率为99.27%,RSD为0.48%(n=6).结论该法操作简便、快速、结果准确,可用于双黄消炎片的质量控制.     

大鼠血浆中牡荆素鼠李糖苷的质量浓度测定

目的建立测定大鼠血浆中牡荆素鼠李糖苷质量浓度的反相高效液相色谱（RP-HPLC）法。方法以四氢呋喃-乙腈-0.5%冰醋酸（20：2.5：77.5）为流动相,血浆样品经简单的甲醇沉淀蛋白后,采用RP-HPLC法测定。结果血浆中牡荆素鼠李糖苷质量浓度的线性范围为0.2～80.0μg/mL,平均相对回收率为89.27%～98.25%,日内和日间精密度的RSD均小于10.79%,最低检测限为50ng/mL。结论建立的RP-HPLC法简便快速、灵敏度高,适用于牡荆素鼠李糖苷的药代动力学研究。     

用HPLC法测定大鼠血浆中吉西他滨的浓度

目的：建立HPLC法测定大鼠血浆中吉西他滨的浓度。方法：采用Phenomenex色谱柱,以5-溴尿嘧啶为内标,流动相为乙腈-0.1%三氟乙酸溶液（3∶97）,流速1.0 mL/min,检测波长268 nm。结果：大鼠血浆中吉西他滨浓度在1-200μg/mL范围内线性关系良好,方法回收率〉97%,提取回收率〉72%,日内、日间RSD均〈6%。结论：本法快速、高效、灵敏,适用于吉西他滨的血药浓度测定。     

用HPLC法测定大鼠血浆和胆汁中芹菜素的浓度

目的：建立HPLC法测定静脉给药后大鼠体内的芹菜素浓度。方法：采用HPLC法,色谱柱为Dikma C18柱,流动相为甲醇：0．2％（V／V）磷酸水溶液-66．5：33．5,检测波长350nm。用该方法测定5只大鼠静脉给药后不同时间点的血浆及胆汁中芹菜素浓度,计算主要药动学参数及胆汁排泄率。结果：血浆药物浓度的标准曲线在0．04～8μg／mL范围内线性关系良好（r=0．9998）,胆汁药物浓度标准曲线在0．25～8μg／mL范围内线性关系良好（r=0．9998）,血浆和胆汁的精密度和方法回收率均良好。芹菜素静脉给药后符合二室模型,消除半衰期为95．2min,胆汁排泄率为5．64％。结论：该方法灵敏、快速、准确,能够用于芹菜素的药动学研究。芹菜素静脉给药后,血浆浓度迅速下降,部分通过胆汁排泄。     

Determination of pinostrobin in rat plasma by LC-MS/MS: application to pharmacokinetics

A rapid and sensitive method for the determination of pinostrobin in rat plasma was developed using liquid chromatography tandem mass spectrometry (LC-MS/MS) for the first time. Isoliquiritigenin was used as an internal standard in rat plasma. Chromatographic separation was performed on an HiQ Sil C₁₈ column with isocratic elution at a flow rate of 1 mL/min. The mobile phase consisted of water and methanol (9:91, v/v) containing 0.1% formic acid. The quantification limit was 10 ng/mL within a linear range of 10-1000 ng/mL (R = 0.9984). The intra- and inter-day assay precision ranged from 3.8-5.3% to 3.2-5.2%, respectively, and the intra- and inter-day assay accuracy was between 93.2-95.1% and 95.5-104.3%, respectively. Our results indicated that the LC-MS/MS method is effective for pharmacokinetic study of pinostrobin in rat plasma.     

Sensitive assay for the determination of fluvastatin in plasma utilizing high-performance liquid chromatography with fluorescence detection

The authors describe a rapid, useful, specific, and very sensitive high-performance liquid chromatographic assay for the determination of fluvastatin (FV) level using atorvastatin as the internal standard (IS). After a simple deproteinization of 1.0 mL of plasma with acetonitrile, the drug and IS were extracted with tert-methyl butyl ether (TMBE). An efficient separation was performed using an 8 mm x 10 cm Nova Pak C(18) 4-microm particle size radial compression cartridge. The mobile phase consisted of an aqueous solution containing 20 mmol/L dibasic sodium dihydrogen phosphate with 1 mmol/L sodium lauryl sulfate adjusted to pH 7 with phosphoric acid and acetonitrile (70:30 v/v) delivered at a flow rate of 1.0 mL/min. The compounds of interest were detected using a fluorescence detector with the excitation wavelength set at 305 nm and the emission at 380 nm. Under these conditions, the retention times for FV and IS were 8.8 and 10.6 minutes, respectively. The concentration of FV in plasma was linear (r > 0.999) for the wide range that was examined (0.5-1,000 ng/mL). The recovery ranged from 88% to 96%. This sensitive, rapid, and simple analytical method gives accurate results over the wide range of concentrations examined. This method is used currently for clinical therapeutic monitoring and pharmacokinetic studies of FV in patients with hypercholesterolemia.     

Development of green bioanalytical hplc method for estimation of irbesartan in rat plasma: Towards greener chromatographic science

Environmental friendly, less toxic and reliable liquid chromatography method for estimation of irbesartan was developed and validated in rat plasma. The chromatographic separation was performed on Hypersil Gold C18 column (4.6 mm × 250 mm, 5 µm), using a mobile phase of 0.5% ortho-phosphoric acid (pH 3.0) and ethanol (65:35 v/v) under isocratic elution with a flow rate of 0.8 mL/min. The column eluent was monitored at 225 nm using PDA detector. The retention time of irbesartan was found to be 4.8 min with excellent peak symmetry. Linearity of the developed method was observed for the drug concentration ranging between 0.2 and 10 μg/mL. Other parameters such as accuracy, precision and recovery were found to be well within the acceptable limits. The method was successfully applied for the estimation of irbesartan in rat plasma and various pharmacokinetic parameters were computed. The proposed method was found to be greener and cost effective than the reported methods in literature, hence, can be used for routine analysis of drug in biological matrix without affecting the environment.     

Bioavailability and pharmacokinetics of alantolactone from Inula helenium in rats following intravenous and oral administrations

Alantolactone, as the principal constituent of Inula Helenium L, has been shown various pharmacologic activities, such as anti-inflammatory and deworming. In the present study, we developed a high performance liquid chromatography (HPLC) method for the determination of alantolactone in rat plasma, and pharmacokinetics of alantolactone was investigated after intravenous and oral administrations to Wistar rats. Separation was achieved on C₁₈ column (4.6 mm×250 mm, 5.0 μm) using a mobile phase consisting of methanol–water (70:30, v/v) at a flow rate of 1.0 mL/min. The wavelength of the ultraviolet detector was set at 239 nm. The excellent linearity was found over a concentration range of 0.08–10 μg/mL (R² = 0.9998).The intra- and inter-day precisions were good, and the RSD was lower than 2.27%. The mean absolute recovery of alantolactone in plasma ranged from 88.09% to 95.57%. After intravenous administration, alantolactone showed rapid systemic clearance (CL (0.11±0.014) L/h/kg) and small volume of distribution (Vd (0.71±0.14) L/kg). The biological half life (t_1/2) was 56.24 min. After oral administration, alantolactone showed rapid oral absorption in rats, with a short T_max of(45.02±0.88) and (45.13±0.39) min for 14 and 28 mg/kg, respectively.The bioavailability of alantolactone in rats was 50.88%, indicating that alantolactone was orally available.     

Development of a sensitive bioanalytical method for the quantification of lacosamide in rat plasma. Application to preclinical pharmacokinetics studies in rats

A sensitive and selective high performance liquid chromatographic (HPLC) method was developed and validated for quantification of lacosamide in rat plasma. A liquid-liquid extraction procedure was optimized to extract lacosamide from rat plasma. Chromatographic separation was accomplished using a reversed phase C18 Hichrom (250×4.6 mm, 5 μm) column with the mobile phase consisting of acetonitrile-phosphate buffer (pH 3.2±0.1; 20 mM) (21:79, v/v) at a flow rate of 1 mL/min. Both intra- and inter day assay precision and accuracy were lower than 15% CV. The lower limit of quantitation was 25 ng/mL for lacosamide and the response was linear in a concentration range from 25 to 10 000 ng/mL. The developed method was successfully used for the preclinical pharmacokinetic study of lacosamide in rats.     

高效液相色谱法测定大鼠血浆中葛根素的质量浓度

目的建立测定大鼠血浆中葛根素质量浓度的高效液相色谱（HPLC）法。方法以pH=3.0的磷酸盐缓冲液-乙腈（82∶18）为流动相,以绿原酸为内标,血浆样品经过三氯乙酸沉淀蛋白萃取后,采用HPLC法测定血浆中葛根素的质量浓度。结果葛根素质量浓度线性范围为0.10～4.00μg/mL,日内和日间精密度的RSD均小于14%,平均相对回收率为87.81%～105.83%,葛根素的检测限为50ng/mL。结论所建立的HPLC法灵敏、准确、快速,可用于葛根素的体内检测。     

RP-HPLC法测定大鼠血浆中双嘧达莫浓度

目的建立大鼠血浆中双嘧达莫的RP-HPLC检测方法。方法采用RP-HPLC法测定大鼠血浆中药物浓度,色谱柱为Diamonsil ODS C18(200mm×4.6mm,5μm),流动相为甲醇-pH6.5磷酸二氢钾缓冲液(60∶40,v/v)。结果在0.10～10.0μg/mL范围内,双嘧达莫与内标峰面积比值与浓度线性关系良好(r=0.997),最低检测限为0.05μg/mL,绝对回收率为84.3%～92.3%,准确度为99.9%～103.1%,日内、日间RSD均<10%。结论本测定方法灵敏、准确、简便,适合于双嘧达莫的药代动力学研究。