HPLC—UV法用于人血浆中罗红霉素的浓度测定及药代动力学和生物等效性研究

目的建立HPLC-UV法测定人血浆中罗红霉素的方法,并探讨罗红霉素的药代动力学和生物等效性。方法采用Diamonsil C18柱（150mm×4．6mm,5μm）,流动相为乙腈：0．01mool磷酸二氢铵=39：61（v／v）,流速1mL／min;以卡马西平为内标,检测波长为210nm。血浆样品用正己烷（含5％的异丙醇）液-液萃取后经C18分离。结果罗红霉素在0．25～16．0mg／L线性关系良好,r=0．999,最低检测限为0．25mg／L。萃取回收率〉70％,方法回收率99．8％～110．5％,批内、批间精密度均〈15％。结论HPLC—UV方法结果准确、灵敏度高,适用于罗红霉素药代动力学和生物等效性研究。     

基于UPLC-DAD-TOF/MS结合HPLC-UV法的麻黄“先煎去沫”样品的化学成分分析

目的建立基于UPLC-DAD-TOF/MS结合HPLC-UV法检测麻黄样品化学成分的方法,以明确麻黄"先煎去沫"样品化学成分间的差异。方法 UPLC-DAD-TOF/MS:Waters ACQUITY UPLC?BEH C18(50 mm×2.1 mm,1.7μm)色谱柱,以甲醇-0.1%甲酸水溶液为流动相梯度洗脱,体积流量0.3 m L/min,柱温40℃,正、负离子模式扫描;HPLC-UV:以十八烷基硅烷键合硅胶为填充剂(150 mm×4.6 mm,5μm),以0.1%磷酸水溶液(含0.05%三乙胺)-乙腈溶液(99∶1)为流动相,等度洗脱,体积流量1 m L/min,检测波长为210 nm,柱温30℃。结果上沫中所含成分较少,去沫下液和全煎煮液中化学成分基本一致。同时,三者均可鉴定出去甲基麻黄碱、去甲基伪麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱5个生物碱类成分和1个羧酸类成分(4-羟基-7-甲氧基-2-喹啉羧酸)。但上沫中生物碱含量极低,而全煎煮液中3种生物碱的含量略高于去沫下液。结论麻黄"先煎去"沫理论可能与生物碱类成分关系不大,但仍需后期进行更深入的研究验证。     

Analysis of Imazaquin in Soybeans by Solid-phase Extraction and High-performance Liquid Chromatography

An analytical method for the determination imazaquin residues in soybeans was developed. The developed liquid/liquid partition and strong anion exchange solid-phase extraction procedures provide the effective cleanup, removing the greatest number of sample matrix interferences. By optimizing mobile-phase pH water/acetonitrile conditions with phosphoric acid, using a C-18 reverse-phase chromatographic column and employing ultraviolet detection, excellent peak resolution was achieved. The combined cleanup and chromatographic method steps reported herein were sensitive and reliable for determining the imazaquin residues in soybean samples. This method is characterized by recovery >88.4%, precision <6.7% CV, and sensitivity of 0.005 ppm, in agreement with directives for method validation in residue analysis. Imazaquin residues in soybeans were further confirmed by high performance liquid chromatography-mass spectrometry (LC-MS). The proposed method was successfully applied to the analysis of imazaquin residues in soybean samples grown in an experimental field after treatments of imazaquin formulation.     

Pharmacokinetics of Furegrelate After Oral Administration to Normal Humans

Furegrelate sodium is a thromboxane synthetase inhibitor with potential for the treatment of various diseases including hypertension, thrombosis, and renal disorders. The absorption and disposition of the parent drug in normal male volunteers have been studied after single- and multiple-dose oral administration. The results from the single-dose study indicate that furegrelate is rapidly absorbed, with a T _max of 1.0–1.7 hr, has an apparent terminal disposition rate constant of 0.12–0.17 hr^–1, and is eliminated primarily by the kidney, with 62–78% of the dose excreted as parent drug. After multiple-dose oral administration for 4.5 days using a b.i.d. dosing regimen, no apparent change in the absorption, disposition, and elimination kinetics is detected and only a slight potential for drug accumulation is observed.     

柴胡的质量评价研究△

目的:建立柴胡的质量评价方法。方法:采用薄层色谱法进行定性鉴别;紫外分光光度法,测定柴胡中总皂苷的含量;利用HPLC法,采用C18色谱柱(4.6mm×250mm,5μm)、乙腈-水为流动相,流速:1.0ml.min-1,检测波长:210nm,测定柴胡中柴胡皂苷a、d的含量。结果:柴胡总皂苷在0.03256～0.1628mg、柴胡皂苷a在0.258～2.580μg、柴胡皂苷d在0.238～2.380μg范围内呈良好的线性关系,r分别为0.9969、0.9996、0.9997;平均回收率:柴胡总皂苷为99.73%,柴胡皂苷a为100.40%,柴胡皂苷d为99.70%;RSD:柴胡总皂苷为2.07%,柴胡皂苷a为1.72%,柴胡皂苷d为1.50%。结论:定性鉴别薄层色谱特征明显,专属性强,本研究建立的紫外分光光度法测定柴胡总皂苷及高效液相法测定柴胡皂苷a、d含量的方法,简单、易行、快速,结果准确可靠,能较全面地控制柴胡的质量,并为在安全剂量范围内正确使用柴胡提供依据。     

基于HPLC-UV和FT-NIR的不同贮藏年限余甘子质量评价与鉴别

目的:探寻不同贮藏年限余甘子有效成分变化规律,为其保存策略提供理论依据。方法:采集7个不同贮藏年限的余甘子材料,高效液相色谱紫外光谱(HPLC-UV)测定没食子酸、柯里拉京、诃黎勒酸、鞣花酸、槲皮素的含量,阐明其主要活性成分累积特征;傅立叶变换近红外光谱(FT-NIR)记录样品整体光谱指纹图谱,偏最小二乘判别(PLS-DA)模型鉴别不同贮藏年限余甘子样品。结果:2015年版《中国药典》指标性成分没食子酸含量最高,其次是鞣花酸与诃黎勒酸,柯里拉京与槲皮素的含量较少;各成分在不同贮藏年限间样品中具有显著性差异(P0.05),没食子酸和槲皮素均在贮藏6年时达最大值,分别为79.36和1.68 mg·g~(-1),贮藏4年样品中诃黎勒酸、柯里拉京、鞣花酸累积最高,分别是18.85,7.97,21.46 mg·g~(-1)。MSC+SG二阶求导(窗口参数为11,多项式次数为3)优化FT-NIR数据,不同贮藏年限样品的分类正确率为84.5%;以最低交叉验证均方根误差为准则,降维光谱数据为若干重要潜在变量并与5种活性成分含量数据融合,鉴别正确率提高到98.8%。结论:基于HPLC-UV和FT-NIR技术,该研究有效阐述不同贮藏年限余甘子5种主要代谢成分累积特征;结合数据融合策略,PLS-DA模型能较好鉴别不同质量样品。该结果可为不同贮藏年限余甘子的质量鉴别及评价提供一定的科学依据。     

Quantification of 4′-geranyloxyferulic acid,a new natural colon cancer chemopreventive agent,by HPLC-DAD in grapefruit skin extract

Oxyprenylated natural products (isopentenyloxy-, geranyloxy- and the less spread farnesyloxy-compounds and their biosynthetic derivatives) represent a family of secondary metabolites that have been consider for years merely as biosynthetic intermediates of the most abundant C-prenylated derivatives. Many of the isolated oxyprenylated natural products were shown to exert in vitro and in vivo remarkable anti-cancer and anti-inflammatory effects. 4′-Geranyloxyferulic acid [3-(4′-geranyloxy-3′-methoxyphenyl)-2-trans-propenoic] has been discovered as a valuable chemopreventive agent of several types of cancer. After development of a high yield and “eco-friendly” synthetic scheme of this secondary metabolite, starting from cheap and non-toxic reagents and substrates, we developed a new HPLC-DAD method for its quantification in grapefruit skin extract. A preliminary study on C18 column showed the separation between GOFA and boropinic acid (having the same core but with an isopentenyloxy side chain), used as internal standard. The tested column were thermostated at 28 ± 1 °C and the separation was achieved in gradient condition at a flow rate of 1 mL/min with a starting mobile phase of H₂O:methanol (40:60, v/v, 1% formic acid). The limit of detection (LOD, S/N = 3) was 0.5 μg/mL and the limit of quantification (LOQ, S/N = 10) was 1 μg/mL. Matrix-matched standard curves showed linearity up to 75 μg/mL. In the analytical range the precision (RSD%) values were ≤2% and the accuracy (bias%) between ±12%. This method was used to evaluate for the first time the presence of this analyte in natural extract of grapefruit. In conclusion, this method showed LOQ values able to selective quantification of this analyte in grapefruit skin extract.     

阿奇霉素在中国健康人体血浆中的药动学研究

OBJECTIVE To study the pharmacokinetics of azithromycin tablet in Chinese healthy volunteers.METHODS 10 healthy volunteers were given a single oral dose of 500mg azithromycin tablet.The plasma concentrations of azithromycin were determined by HPLC-UV.The     

北柴胡皂苷类成分的特征(指纹)图谱研究

目的:通过研究39个柴胡样品的特征(指纹)图谱,建立北柴胡高效液相色谱法(HPLC-UV)的指纹图谱分析方法,提供北柴胡药材质量综合评价体系。方法:样品酸化后HPLC-UV法测定柴胡皂苷类成分的指纹图谱;色谱条件:乙腈-水梯度洗脱,检测波长240nm,流速1.0mL.min-1,柱温30℃;运用SPSS软件分析得到的相似度数据。结果:建立了北柴胡HPLC-UV指纹图谱共有模式,得到不同产地柴胡药材的相似度数据,通过聚类分析将样品分为6大类。结论:可以通过与共有模式比较得到的相似度推测柴胡的种源;建议选用中柴1号和山西左权的柴胡种子作为大面积推广的优良品种;建立的指纹图谱具有较广泛的应用范围,为研究柴胡类药材的指纹图谱分析鉴定提供了较好的科学参考数据。