| HPLC-MS/MS同时测定感冒安颗粒中5种黄酮成分的含量 |
| 投稿时间：2024-03-16 修订日期：2024-06-13 点此下载全文 |
| 引用本文：陈方剑,骆锦前,王志君,胡叶帅,孙煜昕,宋洪杰.HPLC-MS/MS同时测定感冒安颗粒中5种黄酮成分的含量[J].药学实践杂志,2024,42(9):402~406 |
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| 中文摘要:目的 建立HPLC-MS/MS方法测定感冒安颗粒中5 种黄酮成分含量。方法 色谱条件：色谱柱为Kromasil C18柱（4.6 mm×150 mm×4.6 mm,5 μm,100 ?），流动相为甲醇（A）-0.1 %甲酸（B），梯度洗脱（0～20 min，35% A；20～40 min，45% A），流速为1.0 ml/min，柱温为25 ℃；质谱条件：电喷雾电离源（ESI源）负离子扫描，多反应监测（MRM）模式检测。5种黄酮检测的离子对：芦丁m/z 609.1→300.1、金丝桃苷和异槲皮苷m/z 463.0→300.1、槲皮素m/z 301.0→151.0、木犀草素m/z 285.0→132.9。结果 5个成分在一定浓度范围内与峰面积具有良好的线性关系，相关系数r均>0.999 1；平均加样回收率在100.63 %～102.81 %之间，RSD范围在0.67 %～2.07 %。10 批感冒安颗粒中芦丁、金丝桃苷、异槲皮苷、槲皮素和木犀草素的含量测定结果分别为32.23～479.83、0.291～1.825、11.44～20.54、6.32～18.41、3.46～6.51 μg/g。结论 建立的HPLC-MS/MS法灵敏度高、专属性强，适合同时测定感冒安颗粒中5 种黄酮类成分的含量。 |
| 中文关键词:高效液相色谱-串联质谱法 感冒安颗粒 芦丁 金丝桃苷 异槲皮苷 槲皮素 木犀草素 |
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| Simultaneous determination of five flavonoids in Ganmao’an granules by HPLC-MS/MS |
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| Abstract:Objective To develop a high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method for simultaneous determination of five flavonoids in Ganmao’an granules （GMA）. Methods Chromatographic separation was achieved on a Kromasil C18 Column （150 mm× 4.6 mm,5 μm,100 ?）, which was eluted with methanol （A）-0.1 % formic acid （B） at the flow rate of 1.0 ml/min. The gradient condition was as follows: 0-20 min, 35% A, and 20-40 min, 45% A. The column temperature was 25 °C. Analytes were detected using a triple quadrupole tandem mass spectrometer equipped with an electrospray ionization source in the negative ion scanning. The multiple reaction monitoring mode was used for qualitative analysis. For each flavonoid, two precursor ion/product ion transitions were chosen: lutin m/z 609.1→300.1, hyperin and isoquercitrin m/z 463.0→300.1, quercetin m/z 301.0→151.0, luteolin m/z 285.0→132.9. Results Five flavonoids showed the good relationships within their own concentration ranges （correlation coefficient r>0.999 1），whose average recoveries were in the range of 100.63 %-102.81 % with RSDs of 0.67 %-2.07 %. The content results of rutin, hyperoside, isoquercetin, quercetin, and luteolin in 10 batches of GMA were 32.23-479.83, 0.291-1.825, 11.44-20.54, 6.32-18.41, 3.46-6.51 μg/g, respectively. Conclusion The results indicated that the developed method was sensitive, accurate and could provide excellent specificity for simultaneous determination of five flavonoids in GMA. |
| keywords:HPLC-MS/MS Ganmao’an granules rutin hyperin isoquercitrin quercetin luteolin |
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