Determination of lansoprazole in human plasma by rapid resolution liquid chromatography–electrospray tandem mass spectrometry: Application to a bioequivalence study on Chinese volunteers

A simple, sensitive and rapid LC/MS/MS method was developed for the quantification of lansoprazole in human plasma. After a simple sample preparation procedure by one-step protein precipitation with acetonitrile, lansoprazole and the internal standard bicalutamide were chromatographed on a Zorbax SB-C₁₈ (3.0 mm × 150 mm, 3.5 μm, Agilent) column with the mobile phase consisted of methanol–water (70:30, v/v, containing 5 mM ammonium formate, pH was adjusted to 7.85 by 1% ammonia solution). Detection was performed on a triple quadrupole tandem mass spectrometry by multiple reaction monitoring (MRM) mode via negative eletrospray ionization source (ESI⁻). The lower limit of quantification was 5.5 ng/mL, and the assay exhibited a linear range of 5.5–2200.0 ng/mL. The validated method was successfully applied to investigate the bioequivalence between two kinds of preparation (test vs. reference product) in twenty-eight healthy male Chinese volunteers.     

Pharmacokinetics and distribution of schisandrol A and its major metabolites in rats

1.?Schizandrol A is an active component in schisandra, also the representative component for the identification of schisandra.

2.?A rapid resolution liquid chromatography coupled with quadruple–time–of–flight mass spectrometry (RRLC–QTOF/MS) was developed to investigate the pharmacokinetics of schizandrol A after its intragastric administration (50?mg/kg) in rats.

3.?Schizandrol A was rapidly absorbed (T _max = 2.07?h), with a longer duration (t _1/2 = 9.48?h) and larger apparent volume of distribution (Vz/F?=?111.81?l/kg) in rats. Schizandrol A can be detected in main organs and the order of its distribution was in the liver?>?kidney?>?heart?>?spleen?>?brain, particularly higher in the liver.

4.?Five schizandrol A metabolites were identified, including 2–demethyl–8(R)–hydroxyl–schizandrin, 3–demethyl–8(R)–hydroxyl–schizandrin, hydroxyl–schizandrin, demethoxy–schizandrin, 2, 3–demethyl–8(R)–hydroxyl–schizandrin, indicating that the hydroxylation and demethylation may be the major metabolic way of schizandrol A.

5.?This study defined the pharmacokinetic characteristics of schizandrol A in vivo, and the RRLC–QTOF/MS is more sensitive and less limited by conditions, and needs less samples, which may be a useful resource for the further research and development of schisandrol A.     

基于化学计量学的RRLC指纹图谱在川白芷硫熏前后质量控制和识别中的应用

 目的 基于化学计量学的RRLC指纹图谱方法对川白芷硫熏前后进行质量控制和识别。方法 采用Agilent Zorbax SB-C₁₈色谱柱(4.6 mm×100 mm,1.8 μm;以甲醇-水为流动相梯度洗脱,流速1.0 mL·min-1,检测波长310 nm;采用主成分分析、系统聚类分析等方法对川白芷熏硫前后进行质量控制和模式识别。结果 该方法可使川白芷中各成分得到较好的分离,并根据检测结果确定了23个共有指纹峰。川白芷熏硫前后样品的指纹图谱存在较大差异。结论 基于化学计量学的RRLC指纹图谱可对川白芷药材硫熏前后进行质量控制和识别,可为川白芷内在质量控制提供参考。     

Optimization of Supercritical Fluid Extraction and Rapid Resolution LC-MS/ESI Identification of Chromones from Saposhnikoviae Radix through Orthogonal Array Design

Objective To establish a rapid and effective supercritical fluid extraction(SFE) and rapid resolution liquid chromatography method coupled with diode-array detector(RRLC-DAD) to quantify the chromones in a species. Methods The effects of four parameters including ethanol concentration(50%-90%), pressure(25-45 MPa), temperature(40-60 ℃), and time(30-90 min) on the chromones yields, namely prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, and sec-O-glucosylhamaudol, were investigated using SFE system with orthogonal array design(OAD). Furthermore, the extracts were analyzed using rapid resolution liquid chromatography coupled with diode-array detector(RRLC-DAD) system to confirm the results. Results Under the optimized conditions, i.e., 35 MPa of pressure, 60 ℃ of temperature, 70% ethanol, and 60 min of time, the yields of prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, sec-O-glucosylhamaudol, and total chromones were 3.514, 0.132, 6.242, 0.342, and 10.231 mg/g, respectively. In comparison with ultrasonic assisted extraction(UAE), SFE was able to yield a 20.7% increase in the total chromones from Saposhnikoviae Radix. Conclusion SFE is an alternative and promising method to extract chromones from this species, and the established RRLC-DAD method could serve as a rapid and effective method for the identification of chromones from Saposhnikoviae Radix.     

RRLC法同时测定橘红痰咳颗粒中苦杏仁苷和柚皮苷

目的 建立用快速高分离度液相色谱( RRLC)同时测定橘红痰咳颗粒(化橘红、苦杏仁、百部、水半夏、茯苓、白前、五味子、甘草)中苦杏仁苷和柚皮苷的方法.方法 采用BDS HYPERSIL C18(4.6 mm× 100 mm,2.4 μm)色谱柱;流动相为乙腈-0.1％磷酸,梯度洗脱;体积流量为2.0 mL/min;检测波长为207 nm;柱温为30℃;进样体积为2.5 μL.结果 样品中苦杏仁苷、柚皮苷在6min内完全分离并对其进行了定量测定,苦杏仁苷、柚皮苷进样量分别在0.041 68 ～0.4168μg、0.063 06～0.630 6 μg范围内有良好的线性关系(r=0.9999).平均回收率(n=6)分别为99.8％,101.0％:RSD分别为0.5％,1.0％.结论 RRLC法可大幅提高苦杏仁苷和柚皮苷的分析速度,同时减少了溶剂消耗,在多组分复杂体系的快速分析中仍然可以保持出色的分离重现性,可作为传统HPLC方法的一种更新、替代方法.     

UPLC、RRLC及UFLC在中药质量控制中的研究进展

文章综述了近几年来超高效液相色谱(UPLC)、高分离度快速液相色谱(RRLC)和超快速液相色谱(UFLC)在中药成分定性鉴别、含量测定、指纹图谱及中药限量成分或违禁添加成分检测中的研究进展。     

RRLC（高分离度快速液相色谱）法测定孕钙片中叶酸的含量

目的：采用RRLC（高分离度快速液相色谱）仪测定孕钙片中叶酸的含量。方法：色谱柱为Zorbax XDB—C18（4．6×50mm,1．8um）,流动相：乙腈-5％甲酸（31：69）,检测波长：280nm,流速：1．0mL·min^-1,柱温：30℃。结果：叶酸在0．2—1．0μg·ml^-1（r=0．9996）内峰面积与浓度呈良好的线性关系,加样回收率为99．28％（RSD=2．65％）。结论：采用RRLC（高分离度快速液相色谱）仪测定孕钙片中叶酸的含量,可缩短分析时间,提高效率,降低成本。本方法简便、准确,结果稳定。     

RRLC-MS/MS法同时测定保健食品中31种降糖、降压、降血脂类非法添加化学药物

摘 要 目的：建立同时测定保健食品中31种降糖、降压、降血脂类非法添加化学药物的快速液相色谱 串联四级杆质谱（RRLC MS/MS）方法。 方法: 供试品以甲醇为提取溶剂,用甲醇 水（2∶8）稀释,经Agilent ZORBAX Eclipse Plus C18 Rapid Resolution HD色谱柱（50 mm×3.0 mm,1.8 μm）分离,以0.1%的甲酸溶液为流动相A,乙腈 甲醇（1∶1）为流动相B,梯度洗脱。质谱采用ESI源,正负模式同扫,动态多反应监测模式。以保留时间、定性离子对、离子比率进行定性分析,以定量离子对峰面积进行外标法定量分析。 结果: 31种化合物在线性范围内相关性均较好,相关系数均大于0.997 0;平均回收率为95.7%～100.5%,RSD为0.8%～2.7%;检出限在9.6～983.6 ng·g-1之间;单次分析仅需10 min。结论: 该方法专属性较好、灵敏度较高、快速、简便,适应于31种降糖、降压、降血脂类非法添加化学药物的筛查和确证。     

快速分离液相色谱法测定庆大霉素普鲁卡因维B12颗粒中维生素B12的含量

目的 建立快速分离液相色谱（RRLC）法测定庆大霉素普鲁卡因维B12颗粒中维生素B12含量的方法.方法 选用Agilent SB-C18柱（3.0 mm×150 mm,1.8 μm）;以0.005 mol·L-1磷酸二氢钾溶液（每1 000 mL加磷酸0.5 mL）-甲醇（75：25）为流动相;流速为0.5 mL·min-1;柱温40 ℃;检测波长361 nm;进样体积200 μL.结果 VB12在10～1 400 ng· mL-1浓度范围内与峰面积呈良好的线性关系（r=0.999 8,n=9）.平均加样回收率为100.2%（RSD为1.0%,n=6）.方法 的最低检出限为8.0 ng· mL-1.供试品溶液色谱图中VB12峰与相邻峰的分离度良好,样品中其他组分不干扰VB12的测定.结论 该方法快速,简便,重复性好,结果准确可靠,适用于庆大霉素普鲁卡因维B12颗粒中微量维生素B12的含量测定.     

紫草中萘醌类化学成分的快速高效液相色谱-飞行时间质谱联用技术分析

目的:对紫草中萘醌类化学成分进行快速分离与鉴别。方法:采用快速高效液相色谱-飞行时间质谱(RRLC/Q-TOF/MS)法。色谱柱为Agilent SB-C18(100 mm×4.6 mm,1.8μm),流动相为乙腈-0.1%甲酸溶液(梯度洗脱),流速为0.4 ml/min,柱温为30℃;使用甲喷雾离子源,正、负离子扫描模式,载气温度为450℃,质量扫描范围(m/z)为100¹ 000。结果:推断出紫草中可能含有紫草素、β-羟基异戊酰紫草素、乙酰紫草素、β-乙酰氧基异戊酰紫草素、异丁酰紫草素、β,β-二甲基丙烯酰紫草素和α-甲基-正丁酰紫草素等10种化学成分。结论:该方法快速、高效,可为紫草的药效学和质量控制研究奠定基础。