目的 建立高效液相色谱-紫外/质谱(HPLC-UV/MS)联合测定加味逍遥丸中13种主要成分的含量。方法 HPLC采用Agilent SB C18 (4.6 mm×100 mm,1.8 μm)色谱柱;以甲醇(A)、乙腈(B)、体积分数0.1%磷酸水溶液(C)为流动相,梯度洗脱,流速为0.6 mL·min-1;检测波长分别为210 nm(没食子酸、芍药苷、阿魏酸、甘草苷、1,2,3,4,6-O-五没食子酰葡萄糖、丹皮酚、藁本内酯)和254 nm(绿原酸、栀子苷、甘草酸、柴胡皂苷B2)。LC-MS/MS采用Agilent XDB C18 (4.6 mm×50 mm,1.8 μm)色谱柱;以0.1%甲酸水溶液(A)、甲醇-乙腈=1:1(B)为流动相,等度洗脱,流速为0.5 mL·min-1,质谱采用ESI离子源,正/负离子模式,离子对:白术内酯Ⅱ(233.0→150.7)、茯苓酸(527.5→465.2)。结果 加味逍遥丸中13种主要成分在HPLC-UV/MS中线性关系良好,平均加样回收率为92.53%~103.7%,RSD为0.81%~3.06%。结论 所用方法准确可靠、重复性好,可用于加味逍遥丸全面的质量控制。
Abstract
OBJECTIVE To establish a method for determination of 13 main components in Jiawei-xiaoyao pills by high performance liquid chromatography with ultraviolet (HPLC-UV) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). METHODS HPLC-UV determination was performed on an Agilent SB C18 column (4.6 mm×100 mm, 1.8 μm) with mobile phase of methanol (A), acetonitrile (B) and 0.1% phosphoric acid solution (C) at a flow rate of 0.6 mL·min-1 in a gradient elution manner. The detection wavelength was set at 210 nm for gallic acid, paeoniflorin, ferulic acid, liquiritin, 1,2,3,4,6-pentagalloylglucose, paeonol, ligusticolide, and 254 nm for chlorogenic acid, geniposide, glycyrrhizin, saikosaponin B2, respectively. LC-MS/MS determination was performed on an Agilent XDB C18 (4.6 mm×50 mm, 1.8 μm) column with mobile phase of 0.1% formic acid aqueous solution (A) and methanol: acetonitrile=1:1 (B) at a flow rate of 0.5 mL·min-1 in an isocratic elution manner. The mass spectrum was detected by ESI ion source with positive/negative ion modes. The multiple-reaction monitoring (MRM) was utilized for the detection with m/z at 233.0→150.7 for atractylodes Ⅱ and 527.5→465.2 for pachymic acid. RESULTS The linear relationship of the 13 main components in Jiawei-xiaoyao pills was good in the HPLC-UV/MS method. The average recovery of the sample was 92.53%-103.7%, and the RSD was 0.81%-3.06%. CONCLUSION The method established in this study is accurate, reliable, reproducible, and can be used for the overall quality control of Jiawei-xiaoyao pills.
关键词
加味逍遥丸 /
高效液相色谱-紫外/质谱 /
含量测定 /
质量控制
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Key words
Jiawei-xiaoyao pills /
HPLC-UV/MS /
content determination /
quality control
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中图分类号：
R917
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参考文献
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基金
江苏省中医药科技发展计划重点项目资助(ZD202206);河南省科技攻关项目资助(222102310055);河南省中医药科学研究专项课题资助(20-21ZY2307);南京中医药大学自然科学基金面上项目资助(XZR2020015)
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