超高效液相色谱测定前列安通片中的芍药苷含量

目的:采用超高效液相色谱(UPLC)建立前列安通片中芍药苷的检测方法。方法:采用ACQUITY UPLCTMBEHC18(2.1 mm×50 mm,1.7μm)色谱柱,以乙腈-水-醋酸(15:85:0.15)为流动相,流速为0.2 ml/min,检测波长230 nm,芍药苷的保留时间为2.24 min。结果:实验表明,芍药苷浓度在5~100μg/ml范围内呈良好线性关系(r=0.9998),平均回收率为98.0%(n=6)。结论:本方法快速、简单,分离度和灵敏度高,可用于对前列安通片中芍药苷的快速测定。     

Stable dry powder inhaler formulation of tranilast attenuated antigen-evoked airway inflammation in rats

Tranilast (TL) has been clinically used for the treatment of airway inflammatory diseases, although the clinical use of TL is limited because of its poor solubility and systemic side effects. To overcome these drawbacks, a novel respirable powder of TL (CSD/TL-RP) for inhalation therapy was developed using nanocrystal solid dispersion of TL (CSD/TL). Stability study on CSD/TL-RP was carried out with a focus on inhalation performance. Even after 6 months of storage at room temperature, there were no significant morphological changes in micronized particles on the surface of carrier particles as compared with that before storage. Cascade impactor analyses on CSD/TL-RP demonstrated high inhalation performance with emitted dose and fine particle fraction (FPF) of ca. 98% and 60%, respectively. Long-term storage of CSD/TL-RP resulted in only a slight decrease in FPF value (ca. 54%). Inhaled CSD/TL-RP could attenuate antigen-induced inflammatory events in rats, as evidenced by marked reduction of granulocytes in bronchoalveolar lavage fluid and inflammatory biomarkers such as eosinophil peroxidase, myeloperoxidase, and lactate dehydrogenase. These findings were consistent with decreased expression levels of mRNAs for nuclear factor-kappa B and cyclooxygenase-2, typical inflammatory mediators. Given these findings, inhalable TL formulation might be an interesting alternative to oral therapy for the treatment of asthma and other airway inflammatory diseases with sufficient dispersing stability.     

苍耳子中酚酸类化合物的鉴别及绿原酸的含量测定

目的:鉴别苍耳子药材中的酚酸类化合物,比较和分析不同产地苍耳子中绿原酸的含量,建立苍耳子的质量控制方法。方法:根据化合物的紫外光谱、液相色谱保留时间及质谱数据等综合信息鉴别苍耳子药材中的酚酸类成分,采用UPLC对苍耳子中绿原酸的含量进行测定,流动相甲醇-0.1%磷酸水溶液,检测波长为327 nm,流速为0.4 mL.min-1,柱温35℃。结果:对苍耳子药材中的9种酚酸类成分的化学归属进行了指认,并测定了24批苍耳子药材中绿原酸的含量,结果绿原酸在3.5～350 mg.L-1具有良好的线性关系(R2=0.999 9),平均回收率(n=6)为101.7%。结论:苍耳子中特征化学成分的识别可以显著增强其质量控制的准确性和专属性,而快速准确的指标成分含量测定方法,也是苍耳子质量控制的重要检测手段,定性与定量两方面结合,对于苍耳子药材及其相关产品的质量检测和控制具有重要意义。     

高良姜黄酮提取物特征谱分析及成分确认

目的:建立不同批次高良姜提取物的特征谱并进行成分鉴定。方法:采用HPLC分析高良姜提取物的特征指纹谱。SunfireTMC18色谱柱,流动相乙腈-0.1%的甲酸溶液梯度洗脱,分析时间60 min,检测波长208 nm,柱温30℃,流速1.0 mL.min-1。采用超高效液相色谱串联四级杆飞行时间质谱联用技术(UPLC/Q-TOF MS)进行分析,对主要成分进行鉴定。结果:特征谱共标出10个共有峰。鉴定出提取物中12个化合物。结论:采用HPLC特征指纹谱能有效控制高良姜提取物的质量。     

UPLC测定注射用头孢哌酮钠舒巴坦钠

目的:建立超高效液相色谱检测注射用头孢哌酮钠舒巴坦钠含量及有关物质的方法。方法:采用ACQUITY UPLC HSSC18色谱柱,以0.1%磷酸水溶液和乙腈为流动相进行梯度洗脱,流速0.45 mL.min-1,检测波长为220 nm,柱温为30℃。结果:头孢哌酮与舒巴坦在20～150μg.mL-1范围内r≥0.9998,各杂质均呈良好的线性关系;头孢哌酮平均回收率为99.9%,RSD为0.40%;舒巴坦平均回收率为99.5%,RSD为0.36%;重复性、专属性、供试品溶液稳定性良好,各组分之间互相无干扰。结论:该方法专属性强、灵敏度高、准确性好,可以作为注射用头孢哌酮钠舒巴坦钠含量测定及有关物质检查的有效方法。     

Determination of a novel thrombin receptor antagonist (SCH 530348) in human plasma: evaluation of Ultra Performance Liquid Chromatography™-tandem mass spectrometry for routine bioanalytical analysis

SCH 530348 is a safe and effective oral anti-platelet agent for patients with acute coronary syndrome. Clinical study results suggest that SCH 530348 dosage at 20 mg or 40 mg is feasible to achieve rapid maximum platelet inhibition following an acute coronary event or intervention procedure. To permit accurate determinations of circulating SCH 530348 in plasma following dosing, a method for measuring SCH 530348 concentrations in human plasma was validated using liquid chromatography–tandem mass spectrometry (LC–MS/MS). The method utilized semi-automated 96-well protein precipitation with gradient chromatography using an ACQUITY™ UPLC BEH C₁₈ (2.1 mm × 50 mm, 1.7 μm) column. The retention time of SCH 530348 was approximately 1.5 min. This method was validated for routine quantitation of SCH 530348 over the concentration range of 1.00–1000 ng/mL. Inter-run accuracy based on mean percent theoretical for replicate quality control samples was better than 95.2%. Inter-run precision based on percent relative deviation for replicate quality control samples was ≤3.3%. SCH 530348 quality control samples were stable in human plasma for up to three freeze/thaw cycles, for at least 467 days when frozen at −20 °C and for at least 7 h when stored at room temperature. The lower limit of quantitation was 1.00 ng/mL for a 100 μL plasma aliquot.     

UPLC法测定大鼠血浆中Liguzinediol浓度以及动力学研究

目的建立测定大鼠血浆中Liguzinediol浓度的UPLC测定方法,探讨其在大鼠体内的药代动力学。方法血浆样品经甲醇提取后,上清液经N2吹干流动相复溶后注入UPLC分析,色谱柱为UPLC HSS T3柱(2.1 mm×100 mm,1.8μm),流动相为甲醇-水(28∶72,V∶V),流速为0.4 ml.min-1,检测波长278 nm。SD大鼠6只,iv给药10 mg.kg-1后,用UPLC法测定给药后大鼠血浆中Liguzinediol的浓度,利用DAS软件拟合并计算其药代动力学参数。结果 Ligu-zinediol的血药浓度在0.41～52.4 mg.L-1范围内呈线性,提取回收率均>80%,日内、日间精密度<10%,符合生物样品分析要求。大鼠静脉注射10 mg.kg-1的Liguzinediol,其血药浓度(C)-时间(t)曲线呈二室模型,主要药动学参数T12β、AUC(0-∞)、CL分别为1.62 h、18.36 mg.h.L-1、0.71 L.h-1.kg-1。结论该方法操作简便、快速、专属性强,可用于Liguzinediol的药代动力学及成药性研究。     

Development and validation of a stability indicating UPLC method for determination of ticlopidine hydrochloride in its tablet formulation

The objective of the current study was the development of a simple, precise and accurate isocratic reversed-phase stability indicating Ultra Performance Liquid Chromatography [UPLC] assay method and validated for determination of ticlopidine hydrochloride in solid pharmaceutical dosage forms. Isocratic separation was achieved on a Zorbax SB-C18 (50 mm × 4.6 mm, 1.8 μm) column using mobile phase of methanol–0.01 M ammonium acetate buffer, pH 5.0 (80:20, v/v) at a flow rate of 0.8 ml min⁻¹, the injection volume was 4.0 μl and the detection was carried out at 235 nm by using photo-diode array detector. The drug was subjected to oxidation, hydrolysis, photolysis and heat to apply stress condition. The method was validated for specificity, linearity, precision, accuracy, robustness and solution stability. The method was linear in the drug concentration range of 62.5–375 μg ml⁻¹ with a correlation coefficient of 0.9999. The precision (relative standard deviation – RSD) of six samples was 1.31% for repeatability and the intermediate precision [RSD] among six-sample preparation was 0.77%. The accuracy (recovery) was between 98.80% and 101.50%. Degradation products produced as a result of stress studies did not interfere with detection of ticlopidine hydrochloride and the assay can thus be considered stability indicating.     

Validated UPLC method for the fast and sensitive determination of steroid residues in support of cleaning validation in formulation area

An ultra performance liquid chromatographic (UPLC) method was developed for simultaneous determination of seven steroid (dienogest, finasteride, gestodene, levonorgestrel, estradiol, ethinylestradiol, and norethisterone acetate) active pharmaceutical ingredient (API) residues. A new, generic method is presented, with which it is possible to verify the cleaning process of a steroid producing equipment line used for the production of various pharmaceuticals. The UPLC method was validated using an UPLC™ BEH C18 column with a particle size of 1.7 μm (50 mm × 2.1 mm) and acetonitrile–water (48:52, v/v) as mobile phase at a flow rate of 0.55 ml/min. Method development and method validation for cleaning control analysis are described. The rapid UPLC method is suitable for cleaning control assays within good manufacturing practices (GMP) of the pharmaceutical industry.     

Monitoring healthy metabolic trajectories with nutritional metabonomics

Metabonomics is a well established analytical approach for the analysis of physiological regulatory processes via the metabolic profiling of biofluids and tissues in living organisms. Its potential is fully exploited in the field of "nutrimetabonomics" that aims at assessing the metabolic effects of active ingredients and foods in individuals. Yet, one of the greatest challenges in nutrition research is to decipher the critical interactions between mammalian organisms and environmental factors, including the gut microbiota. "Nutrimetabonomics" is today foreseen as a powerful approach for future nutritional programs tailored at health maintenance and disease prevention.