高效液相色谱波长切换法同时测定甲亢灵片中4种成分的含量  

Simultaneous determination of four ingredients in Jiakangling tablets by HPLC wavelength switching method

作　　者：洪强 何胜利 

机构地区：[1]武汉市蔡甸区中医医院,湖北武汉430100 [2]遂成药业股份有限公司,河南新郑451150

出　　处：《安徽医药》2017年第4期639-642,共4页Anhui Medical and Pharmaceutical Journal

摘　　要：目的建立高效液相色谱(HPLC)波长切换法,同时测定甲亢灵片中去甲蟛蜞菊内酯、蟛蜞菊内酯、乌索酸和迷迭香酸含量。方法采用Kromasil C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇(A)-0.5%冰醋酸溶液(B),梯度洗脱;柱温为30℃;进样量为10μL;流速为1.0 mL·min-1;去甲蟛蜞菊内酯和蟛蜞菊内酯检测波长为λ1=351 nm,乌索酸检测波长为λ2=210 nm,迷迭香酸检测波长为λ3=330 nm。结果去甲蟛蜞菊内酯、蟛蜞菊内酯、乌索酸和迷迭香酸在35 min内得到较好的分离,在给定浓度范围内与峰面积呈现良好线性,分别为5.90~118.00 mg·L^(-1)(r=0.999 5)、5.37~107.40 mg·L^(-1)(r=0.999 7)、5.04~100.80 mg·L^(-1)(r=0.999 6)、7.65~153.00 mg·L^(-1)(r=0.999 3);平均加样回收率(n=6)和RSD值分别为98.6%(1.39%)、96.8%(0.83%)、99.2%(1.02%)、97.4%(0.85%)。结论建立的HPLC方法可同时测定甲亢灵片中去甲蟛蜞菊内酯、蟛蜞菊内酯、乌索酸和迷迭香酸含量,方法简便、重现性好、灵敏度高,可用于甲亢灵片中去甲蟛蜞菊内酯、蟛蜞菊内酯、乌索酸和迷迭香酸的含量测定。Objective To establish an HPLC method for simultaneously determining the contents of isodemethyl wedelolactone,wedelo- lac-tone, ursolic acid and rosmarinic acid in Jiakangling tablets. Methods A stable HPLC method was established and the chromatog-raphy method was accomplished on a Kromasil C18 column （250 mm ×4. 6 mm,5 μm） ,with a mobile phase consisting of methanol （A）-0.5% acetic acid （B） with gradient elution;the column temperature was at 30 ;all the injection volume was 10 μL;the flow rate was 1.0 mL ·min^-1 ;isodemethyl wedelolactone and wedelolac-tone were detected at 351 nm,ursolic acid was detected at 210 nm, rosmarinic acid was detected at 330 nm. Results Isodemethyl wedelolactone,wedelolac-tone,ursolic acid and rosmarinic acid had good separation in 35 min. They showed good linearity in the given concentration range at 5. 90-118. 00 mg · L^-1 （ r = 0. 999 5） ,5. 37-107. 40 mg · L^-1 （ r = 0. 999 7） ,5. 04-100. 80 mg · L^-1 （ r = 0. 999 6 ） ,7. 65-153. 00 mg · L^-1（ r = 0. 999 3 ） , respectively. The average recoveries （n =6） and RSD were 98. 6% （ 1 . 39% ） ,96. 8% （0 .8 3% ） ,99. 2% （1 .0 2% ） ,9 7 .4% （0. 85% ） , respectively.Conclusions This HPLC method could simultaneously determine the contents of isodemethyl wedelolactone,wedelolac-tone, ursolic acid and rosmarinic acid in Jiakangling tablets. The method is simple, sensitive and reliable, which can be used as a quantitative analy-sis method of isodemethyl wedelolactone,wedelolac-tone,ursolic acid and rosmarinic acid for Jiakangling tablets.

关 键 词：高效液相色谱法 甲亢灵片 去甲蟛蜞菊内酯 蟛蜞菊内酯 乌索酸 迷迭香酸 

分 类 号：O657.72[理学—分析化学] R286.0[理学—化学]