UPLC同时测定复方守宫散中核苷类含量

目的 建立UPLC法同时测定复方守宫散中腺嘌呤、腺苷含量的方法。方法 用Acquity BEH C18(2.1 mm×100 mm,1.7 μm),甲醇-水为流动相,梯度洗脱,流速0.25ml/min,柱温26℃,检测波长254nm。结果 腺嘌呤、腺苷的进样量分别在0.0409~0.5115μg(r=0.9999)、0.0578~0.7220μg(r=0.9996)范围内与其峰面积呈良好的线性关系;平均回收率分别为92.83%、94.90%,RSD分别为1.11%、1.70%。结论 该方法快速、可靠、准确,可作为复方守宫散的质量控制方法。     

UPLC法测定氨苄西林有关物质

目的建立超高效液相色谱检测氨苄西林有关物质的方法。方法采用Acquity UPLC HSS C18色谱柱,以含有冰醋酸、磷酸二氢钾水溶液和乙腈的不同比例的混合液为流动相进行梯度洗脱,流速为0.5 mL·min-1,检测波长为254 nm,柱温为35℃,进样量为5μL。结果氨苄西林在0.272 1³2.652μg·mL-1范围内r≥0.9999;该方法专属性,重复性,耐用性,溶液稳定性良好。各组分间相互无干扰,与HPLC具有同等的检测能力。结论该方法专属性强,灵敏度高,效率较高,可作为氨苄西林有关物质的检测有效方法。     

UPLC法同时测定盐酸阿糖胞苷原料药的含量和有关物质

目的:建立同时测定盐酸阿糖胞苷原料药的含量和有关物质的方法。方法:采用超高效液相色谱法。色谱柱为Inertsil ODS-3 C18,流动相为磷酸盐缓冲液-甲醇(梯度洗脱),流速为0.8 ml/min,检测波长为254 nm,柱温为40Ⅴ,进样量为10μl。结果:尿嘧啶、尿苷、阿糖尿苷、盐酸阿糖胞苷检测质量浓度分别在0.100 8²0.16、0.120.16、0.1²0.12、0.095 620.12、0.095 6¹9.12、0.119.12、0.1²0.004μg/ml范围内与各自峰面积积分值呈良好的线性关系(r=0.999 9、0.999 8、0.999 9、0.999 9);精密度、稳定性、重复性试验的RSD≤0.79%;尿嘧啶、尿苷、阿糖尿苷平均加样回收率为103.8%、102.2%、99.7%,RSD分别为2.44%、2.69%、3.16%(n=9)。结论:该方法准确、灵敏度高、专属性强、重复性好,可用于盐酸阿糖胞苷原料药的质量控制。     

芪归糖痛宁颗粒的UPLC指纹图谱研究

目的:建立芪归糖痛宁颗粒的UPLC指纹图谱。方法:色谱柱为Acquity BEH C18(100 mm×2.1 mm,1.7μm),流动相为乙腈-0.05%磷酸水溶液(梯度洗脱),柱温为26Ⅰ,流速为0.25 ml/min,检测波长为254 nm。利用《中药色谱指纹图谱相似度评价系统》(2004A版)对10批样品的相似度进行评价。结果:芪归糖痛宁颗粒的UPLC指纹图谱共有13个共有峰,方法测定的重复性、精密度和稳定性良好;10批样品的相似度均>0.99。结论:所建指纹图谱可用于芪归糖痛宁颗粒的质量控制。     

UPLC法测定养血清脑颗粒中咖啡酸和阿魏酸的含量

目的建立同时测定养血清脑颗粒中咖啡酸和阿魏酸含量的方法。方法采用ACQUITY UPLC系统,使用ACQUITY BEH C18（2.1mm×100mm,1.7μm）色谱柱,流动相为0.1%乙酸水溶液-甲醇,梯度洗脱,流速0.4m L·min^-1,检测波长325nm,柱温为40℃。结果咖啡酸质量浓度在0.484~24.20ng·m L^-1内与峰面积呈良好的线性关系（r=0.9996）,平均回收率为101.7%（RSD=1.64%,n=6）;阿魏酸质量浓度在1.102~55.10ng·m L^-1内与峰面积呈良好的线性关系（r=0.9997）,平均回收率为100.1%（RSD=1.83%,n=6）。结论建立的方法简便、准确、重复性好,可用于养血清脑颗粒的质量控制,且不同批次养血清脑颗粒中2种酚酸含量基本一致。     

超高效液相色谱法测定热炎宁颗粒中大黄素、咖啡酸、绿原酸、野黄芩苷、木犀草素和虎杖苷

目的：建立超高效液相色谱（UPLC）同时测定热炎宁颗粒中大黄素、咖啡酸、绿原酸、野黄芩苷、木犀草素、虎杖苷6种成分的方法。方法采用UPLC法,Acquity UPLC HSS C18色谱柱（100 mm×2.1 mm,1.7μm）;流动相为[甲醇–乙腈（35∶65）]–0.1%磷酸水溶液为流动相,梯度洗脱,体积流量0.5 mL/min,分段变波长测定,柱温35℃;进样量1.0μL。结果6种成分在选定的范围内线性关系良好（r≥0.9993）;平均加样回收率在99.08%～102.31%,RSD值均小于2.53%（n=6）。结论采用UPLC法对热炎宁颗粒中大黄素、咖啡酸、绿原酸、野黄芩苷、木犀草素、虎杖苷6种成分进行测定,方法操作快速,高效,准确,可用于热炎宁颗粒的质量控制。     

淫羊藿中化学成分的UPLC/Q-TOF-MS分析

目的建立淫羊藿Epimedium brevicornu中化学成分的超高压液相色谱–飞行时间质谱(UPLC/Q-TOF-MS)的分析方法。方法 Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm),流动相为0.1%甲酸水溶液–乙腈,梯度洗脱;体积流量为0.4 mL/min;柱温为45℃;进样量为2μL。质谱检测采用正、负离子模式,电压分别为3.0、2.5 kV;离子源温度110℃;雾化温度400℃;雾化气体积流量800 L/h。结果在10 min内完成淫羊藿中40个化学成分的鉴定。结论建立了一种简单、快速、高效的UPLC/Q-TOF-MS方法对淫羊藿中化学成分进行了鉴定,为全面控制淫羊藿的质量和机理研究提供了基础。     

Metabolic profiling of isomeric aglycones central‐icaritin (c‐IT) and icaritin (IT) in osteoporotic rats by UPLC‐QTOF‐MS

The isomers, although of similarly chemical structures, have different pharmacological activities due to their metabolic processes in vivo. Central‐icaritin (c‐IT) and icaritin (IT) are isomers and major bioactive aglycones of the Herba Epimedii. In this study, we found that the anti‐osteoporotic effect of c‐IT was stronger than IT on bone structural changes in osteoporotic rats evaluated by Micro‐μCT with the parameters of bone mineral density (BMD), bone mineral content (BMC), tissue mineral content (TMC), and tissue mineral density (TMD). c‐IT treatment significantly increased the bone microarchitecture, compared with IT (p < 0.05). In order to explain their differences in anti‐osteoporosis, the metabolic profiling and pathways of c‐IT and IT in the plasma, bile, urine, and faeces of ovariectomized (OVX) rats were investigated by ultra‐performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC‐QTOF‐MS) after oral administration of c‐IT or IT (80 mg/kg). Finally, 59 metabolites of c‐IT and 43 metabolites of IT were identified by elucidating their corresponding quasimolecular ions and fragment ions. IT could be quickly absorbed into blood and reached a maximum plasma concentration, and then be rapidly conversed to its glucuronidation metabolites, most of which were excreted out by urine. Interestingly, the absorbed and conjugated speeds of c‐IT were slower than IT. The metabolic processes of c‐IT existed enterohepatic circulation, which decreased the metabolism and excretion rate of c‐IT, and prolonged the anti‐osteoporosis effect. Our findings provided evidence on the difference on metabolic profiles of c‐IT and IT in osteoporotic rats, which might shed new lights on improving anti‐osteoporotic effects of IT and c‐IT. Copyright © 2014 John Wiley & Sons, Ltd.     

UPLC–MS/MS for the determination of azilsartan in beagle dog plasma and its application in a pharmacokinetics study

The purpose of the study is to develop an ultra performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS) to determinate the concentration of azilsartan in the dog plasma. After precipitated by methanol, the plasma sample containing azilsartan and diazepam (internal standard, IS) was determined by UPLC–MS/MS. The mobile phase consisted of acetonitrile-water was pumped at a flow rate of 0.3 ml/min in gradient elution. Kinetex 2.6 μ XB-C18 column (50 × 2.1 mm, 100 Å; Phenomenex, USA) were used for LC separations. The column temperature was 30 °C and the injection volume was 5 μl. The electrospray ionization (ESI) and multiple reaction monitoring (MRM) were applied at the transitions of m/z 457 → 279 (azilsartan) and m/z 285 → 193 (diazepam), respectively. The developed method was identified a good linearity over a concentration range of 2.5–5000 ng/ml. The lower limit of quantitation (LLOQ) was 2.5 ng/ml. The intra-day and inter-day precision (relative standard deviation, RSD%) were less than 10% and accuracy (relative error, RE %) was less than 5% at three quality control levels. The extraction recovery of azilsartan at three quality control levels were 82.41 ± 0.68%, 98.66 ± 11.00%, 102.43 ± 0.82%. And the recovery for IS (100 ng/ml) was 91.75 ± 0.54%. A validated UPLC–MS/MS method was firstly developed for the quantification of azilsartan in dog plasma and it was applied to the pharmacokinetics study.     

超高效液相色谱法在药物有关物质分析中的应用

药物有关物质的控制是药品安全、有效的重要保障,是评价药品质量优劣的关键指标。近年来,超高效液相色谱法在药物有关物质分析领域的应用逐渐增多,如：测定原料药、制剂的有关物质,同时测定药物的含量和有关物质等。