机构地区:[1]浙江中医药大学药学院,浙江杭州310053 [2]厦门大学药学院,福建厦门361102
出 处:《中草药》2022年第10期3006-3013,共8页Chinese Traditional and Herbal Drugs
基 金:国家自然科学基金资助项目(82174096);校级科研基金(国家自然科学基金预研专项)资助项目(2019ZG37)。
摘 要:目的建立三七总皂苷(Panax notoginseng saponins,PNS)传递体(transfersomes,TFSs)(PNS-TFSs)中5种皂苷类成分含量与包封率的测定方法,并探讨药物包封特性。方法采用超高效液相色谱(UPLC)法测定PNS-TFSs制剂中三七皂苷R_(1)(NGR_(1))、人参皂苷Rg_(1)(GRg_(1))、人参皂苷Re(GRe)、人参皂苷Rb_(1)(GRb_(1))与人参皂苷Rd(GRd)的含量,色谱柱为Hypersil Gold柱(100 mm×2.0 mm,1.9μm),流动相为乙腈-水,梯度洗脱,检测波长为203 nm,柱温为28℃。以离心超滤法结合UPLC测定传递体包封率。结果NGR_(1)、GRg_(1)、GRe、GRb_(1)与GRd对应的各色谱峰专属性与分离度良好(R≥1.5),且分别在4.04~505.00、3.98~498.00、4.03~504.00、3.99~499.00、4.00~500.00μg/mL呈良好的线性关系(r≥0.9997),精密度(RSD≤2.40%)、准确度(97.23%≤回收率≤104.50%)与供试品溶液稳定性(RSD≤0.90%)均符合要求;测得PNS传递体中NGR_(1)、GRg_(1)、GRe、GRb_(1)与GRd质量浓度依次为98.14、380.80、41.68、317.50、75.61μg/mL,包封率依次为75.48%、69.68%、69.51%、92.35%、95.97%。结论UPLC法与离心超滤法可用于PNS传递体中多成分含量与包封率的测定,方法快速、准确、可靠。Objective To develop methods for the determination of contents and encapsulation efficiencies of five saponins in Panax notoginseng saponins(PNS)transfersomes(PNS-TFSs)and probe the drug encapsulation features.Methods UPLC was adopted to determine the contents of notoginsenoside R_(1)(NGR_(1)),ginsenoside Rg_(1)(GRg_(1)),ginsenoside Re(GRe),ginsenoside Rb_(1)(GRb_(1))and ginsenoside Rd(GRd)in the preparation of PNS-TFSs.An Hypersil Gold column(100 mm×2.0 mm,1.9μm)was used to separate the analytes with acetonitrile-water mixture as the mobile phase in gradient elution mode,and the detection wavelength was set at 203 nm,the column temperature was 28℃.Encapsulation efficiencies were determined by centrifugal ultrafiltration method combined with UPLC.Results The specificity and resolution(R≥1.5)of the peaks corresponding to each analyte met requirements of methodology.The calibration curves were linear(r≥0.9997)and in the ranges of 4.04—505.00,3.98—498.00,4.03—504.00,3.99—499.00,4.00—500.00μg/mL for NGR_(1),GRg_(1),GRe,GRb_(1) and GRd respectively.RSD(≤2.4%)of repeated measurements with working solution of chemical reference substances(CRS)and recoveries(97.23%—104.50%)of the analytes from the blank transfersomes spiked with their CRS demonstrated respectively the precision and accuracy of the method.The test solutions were stable(RSD≤0.90%)in 12 h.The contents of NGR_(1),GRg_(1),GRe,GRb_(1) and GRd in the transfersomes were 98.14,380.80,41.68,317.50,75.61μg/mL,and their encapsulation efficiencies were 75.48%,69.68%,69.51%,92.35%,95.97%,respectively.Conclusion UPLC is fast,accurate,precise and applicable to the determination of the contents of NGR_(1),GRg_(1),GRe,GRb_(1) and GRd in the transfersomes and the centrifugal ultrafiltration method coupled with UPLC is applicable to the determination of their encapsulation efficiencies.
关 键 词:三七总皂苷 传递体 超高效液相色谱 离心超滤法 包封率 包封特性 三七皂苷R_(1) 人参皂苷Rg_(1) 人参皂苷RE 人参皂苷Rb_(1) 人参皂苷RD
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