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A sensitive HPLC-FLD method for the quantification of 6-O-demethylmenisporphine isolated from Menispermi Rhizoma in rat plasma
Journal of Analytical Science and Technology ( IF 2.4 ) Pub Date : 2021-01-04 , DOI: 10.1186/s40543-020-00255-1
Jinxia Wei , Jia Shao , Yanan Li , Yubo Li

Background To investigate the pharmacokinetics of 6- O -demethylmenisporphine, an oxoisoaporphine alkaloid with significant anti-tumor activities and isolated from Menispermi Rhizoma, a novel and sensitive HPLC assay was established for 6- O -demethylmenisporphine quantification in rat plasma. Methods Peak responses were detected by a highly selective and sensitive fluorescence detector with 426-nm excitation and 514-nm emission wavelengths. Curcumin was employed as the internal standard (IS). A Capcell Pak C 18 column (150 mm × 4.6 mm i.d., 5 μm) and an isocratic elution procedure with a flow rate of 1.0 mL/min were used to exclude the endogenous interfering substance. Acetonitrile-water (68:32, v/v) containing 1% formic acid was employed as mobile phase. A 7-point calibration curve that covered the concentration range of 10–2500 ng/mL was constructed. Results A good linearity was observed with a correlation coefficient ( r ) of 0.9993. The lower limit of quantification for 6- O -demethylmenisporphine was 10 ng/mL. The mean recoveries of analyte in rat plasma exceeded 80.5%. The precision at four concentration levels was within 11.3% and the accuracy ranged from − 7.6 to 6.7%. Conclusion Using this new HPLC-FLD method, the investigation of plasma samples from rats following oral dosing of neat compound and Menispermi Rhizoma extract was successfully conducted. The results will provide a reference for the evaluation of preclinical safety of 6- O -demethylmenisporphine.

中文翻译:

一种灵敏的 HPLC-FLD 方法,用于定量从大鼠血浆中的防黄素中分离的 6-O-去甲基甲萘醌

背景 为了研究 6-O-去甲基甲萘醌(一种具有显着抗肿瘤活性的氧代异皂甙类生物碱并从防黄素中分离出来)的药代动力学,建立了一种新颖且灵敏的 HPLC 检测方法,用于定量大鼠血浆中的 6-O-去甲基甲萘醌。方法通过具有 426 nm 激发波长和 514 nm 发射波长的高选择性和灵敏荧光检测器检测峰值响应。姜黄素用作内标 (IS)。Capcell Pak C 18 色谱柱(150 mm × 4.6 mm 内径,5 μm)和流速为 1.0 mL/min 的等度洗脱程序用于排除内源性干扰物质。含有 1% 甲酸的乙腈-水 (68:32, v/v) 用作流动相。构建了涵盖 10–2500 ng/mL 浓度范围的 7 点校准曲线。结果 观察到良好的线性,相关系数 (r) 为 0.9993。6-O-去甲基甲萘醌的定量下限为 10 ng/mL。大鼠血浆中分析物的平均回收率超过 80.5%。四个浓度水平的精密度在 11.3% 以内,准确度范围为 - 7.6 至 6.7%。结论 使用这种新的 HPLC-FLD 方法,成功地对口服纯化合物和防汗提取物后的大鼠血浆样品进行了研究。研究结果将为6-O-去甲基甲萘醌的临床前安全性评价提供参考。6-O-去甲基甲萘醌的定量下限为 10 ng/mL。大鼠血浆中分析物的平均回收率超过 80.5%。四个浓度水平的精密度在 11.3% 以内,准确度范围为 - 7.6 至 6.7%。结论 使用这种新的 HPLC-FLD 方法,成功地对口服纯化合物和防汗提取物后的大鼠血浆样品进行了研究。研究结果将为6-O-去甲基甲萘醌的临床前安全性评价提供参考。6-O-去甲基甲萘醌的定量下限为 10 ng/mL。大鼠血浆中分析物的平均回收率超过 80.5%。四个浓度水平的精密度在 11.3% 以内,准确度范围为 - 7.6 至 6.7%。结论 使用这种新的 HPLC-FLD 方法,成功地对口服纯化合物和防汗提取物后的大鼠血浆样品进行了研究。研究结果将为6-O-去甲基甲萘醌的临床前安全性评价提供参考。成功地对口服纯化合物和防汗提取物后的大鼠血浆样品进行了研究。研究结果将为6-O-去甲基甲萘醌的临床前安全性评价提供参考。成功地对口服纯化合物和防汗提取物后的大鼠血浆样品进行了研究。研究结果将为6-O-去甲基甲萘醌的临床前安全性评价提供参考。
更新日期:2021-01-04
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