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引用本文:张晓景,王英瑛,李俊.多波长HPLC梯度洗脱法同时测定眠安宁合剂中7个有效成分含量[J].中国现代应用药学,2015,32(2):194-198.
ZHANG Xiaojing,WANG Yingying,LI Jun.Simultaneous Determination of Seven Active Components in Mian’anning Mixture by HPLC Under Multiple UV Wavelengths[J].Chin J Mod Appl Pharm(中国现代应用药学),2015,32(2):194-198.
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多波长HPLC梯度洗脱法同时测定眠安宁合剂中7个有效成分含量
张晓景1, 王英瑛2, 李俊2
1.浙江省温岭市食品药品检验检测中心,浙江 温岭 317500;2.浙江省台州市食品药品检验所,浙江 台州 318000
摘要:
目的 建立多波长高效液相梯度洗脱法同时测定眠安宁合剂中5-羟甲基糠醛、远志(口山)酮Ⅲ、白术内酯Ⅰ、白术内酯Ⅲ、丹酚酸B、丹参酮ⅡA、梓醇7个成分的含量。方法 采用依利特Hypersil C18色谱柱(4.6 mm×250 mm,5 μm);流速:0.7 mL·min-1;流动相A为甲醇-乙腈(1∶3),流动相B为0.1%磷酸水溶液,梯度洗脱;检测波长:5-羟甲基糠醛为284 nm,远志(口山)酮Ⅲ为320 nm,白术内酯Ⅰ和白术内酯Ⅲ为220 nm,丹酚酸B和丹参酮ⅡA为270 nm,梓醇为210 nm,柱温为25 ℃。结果 5-羟甲基糠醛、远志(口山)酮Ⅲ、白术内酯Ⅰ、白术内酯Ⅲ、丹酚酸B、丹参酮ⅡA和梓醇质量浓度分别在10.08~100.80 μg·mL-1(r=0.999 8)、3.55~35.50 μg·mL-1(r=0.999 3)、5.80~58.00 μg·mL-1(r=0.999 1)、4.20~42.00 μg·mL-1(r=0.999 9)、40.50~405.00 μg·mL-1(r=1.000)、12.28~122.80 μg·mL-1(r=0.999 5)、7.90~79.00 μg·mL-1(r=0.999 9)内与其峰面积呈良好的线性关系;5-羟甲基糠醛、远志(口山)酮Ⅲ、白术内酯Ⅰ、白术内酯Ⅲ、丹酚酸B、丹参酮ⅡA和梓醇的平均加样回收率分别为98.56%,96.94%,99.61%,97.54%,100.04%,98.59%,99.81%,RSD分别为0.97%,1.73%,1.03%,1.35%,0.86%,1.70%,1.43%(n=6)。结论 建立的方法准确可靠,可用于眠安宁合剂的含量控制。
关键词:  眠安宁合剂  5-羟甲基糠醛  远志(口山)酮Ⅲ  白术内酯Ⅰ  白术内酯Ⅲ  丹酚酸B  丹参酮ⅡA  梓醇
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Simultaneous Determination of Seven Active Components in Mian’anning Mixture by HPLC Under Multiple UV Wavelengths
ZHANG Xiaojing1, WANG Yingying2, LI Jun2
1.Zhejiang Wenling Food and Drug Inspection Center, Wenling 317500, China;2.Zhejiang Taizhou Institute for Food and Drug Control, Taizhou 318000, China
Abstract:
OBJECTIVE To develop an HPLC method with multiple wavelength ultraviolet for the simultaneous determination the content of 5-hydroxymethyl-2-furaldehyde, polygalaxanthone Ⅲ, atractylenolide Ⅰ, atractylenolide Ⅲ, salvianolic acid B, tanshinone ⅡA and catalpol in Mian’anning mixture. METHODS The sample was separated on a Hypersil C18 column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of methanol-acetonitrile(1∶3) and 0.1% phosphoric acid solution. The flow rate was 0.7 mL·min-1. The detection wavelength was set at 284 nm for 5-hydroxymethyl-2-furaldehyde, 320 nm for polygalaxanthone Ⅲ, 220 nm for atractylenolide Ⅰ and atractylenolide Ⅲ, 270 nm for salvianolic acid B and tanshinone ⅡA, 210 nm for catalpol. The column temperature was 25 ℃. RESULTS The calibration curves of 5-hydroxymethyl-2-furaldehyde, polygalaxanthone Ⅲ, atractylenolide Ⅰ, atractylenolide Ⅲ, salvianolic acid B, tanshinone ⅡA and catalpol were linear in the range of 10.08-100.80 μg·mL-1(r=0.999 8), 3.55-35.50 μg·mL-1(r=0.999 3), 5.80-58.00 μg·mL-1(r=0.999 1), 4.20-42.00 μg·mL-1(r=0.999 9), 40.50-405.00 μg·mL-1(r=1.000), 12.28-122.80 μg·mL-1(r=0.999 5), 7.90-79.00 μg·mL-1(r=0.999 9), and the average recoveries(n=6) were 98.56%(RSD=0.97%), 96.94%(RSD=1.73%), 99.61% (RSD=1.03%), 97.54%(RSD=1.35%), 100.04%(RSD=0.86%), 98.59%(RSD=1.70%), 99.81%(RSD=1.43%), respectively. CONCLUSION The method is feasible, accurate and stable, which can control the quatity of Mian’anning Mixture.
Key words:  Mian’anning mixture  5-hydroxymethyl-2-furaldehyde  polygalaxanthone Ⅲ  atractylenolide I  atractylenolide Ⅲ  salvianolic acid B  tanshinone ⅡA  catalpol
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