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目的 建立一测多评法同时测定抗病毒口服液中(R,S)告依春、芒果苷、连翘酯苷I、连翘苷、连翘酯苷A、松脂素吡喃葡萄糖苷和连翘脂素7个成分的含量。方法 采用高效液相色谱法测定,采用Hydrosphere C18色谱柱(4.6mm×250 mm, 5µm);以乙腈(A)0.01%磷酸溶液(B)为流动相梯度洗脱;检测波长为236nm;进样量10 µL。以连翘苷为内参物,计算(R,S) 告依春、芒果苷、连翘酯苷I、连翘酯苷A、松脂素吡喃葡萄糖苷和连翘脂素的相对校正因子和含量,比较外标法和一测多评法的结果差异。结果 7种成分的色谱峰面积与质量浓度呈良好的线性关系,相关系数均大于0.999; 样品加标平均回收率分别 为95.83%~100.27%;测定结果的相对标准偏差为0.11%~2.02%(n=6)。结论本研究建立的抗病毒口服液中7个成分的含量的测定方法准确,简单可行,可用于抗病毒口服液的质量控制。
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| 成分 | 回归方程 | | 线性范围 |
| (R, S)- 告依春 | $Y = {73451X} + {20207}$ | 0.9997 | 0.2402~60.55 |
| 芒果苷 | $Y = {40705X} - {9858.5}$ | 0.9995 | 0.2395~59.878 |
| 连翘酯苷 I | $Y = {10293X} + {1779.4}$ | 0.9998 | 4.90~98.00 |
| 连翘酯苷 A | $Y = {12209X} - {5695.4}$ | 0.9998 | 6.3050 ~1261.0 |
| 松脂素吡喃葡 糖糖苷 | $Y = {13906X} - {5259.9}$ | 0.9994 | 3.92~78.40 |
| 连翘苷 | $Y = {18780X} + {4424.3}$ | 0.9996 | 0.1957 ~48.921 |
| 连翘酯素 | $Y = {25500X} + {358.27}$ | 0.9999 | 0.2417 % 60.417 |
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各成分回归方程, figureFileSmall=null, figureFileBig=null, tableContent=
| 成分 | 回归方程 | | 线性范围 |
| (R, S)- 告依春 | $Y = {73451X} + {20207}$ | 0.9997 | 0.2402~60.55 |
| 芒果苷 | $Y = {40705X} - {9858.5}$ | 0.9995 | 0.2395~59.878 |
| 连翘酯苷 I | $Y = {10293X} + {1779.4}$ | 0.9998 | 4.90~98.00 |
| 连翘酯苷 A | $Y = {12209X} - {5695.4}$ | 0.9998 | 6.3050 ~1261.0 |
| 松脂素吡喃葡 糖糖苷 | $Y = {13906X} - {5259.9}$ | 0.9994 | 3.92~78.40 |
| 连翘苷 | $Y = {18780X} + {4424.3}$ | 0.9996 | 0.1957 ~48.921 |
| 连翘酯素 | $Y = {25500X} + {358.27}$ | 0.9999 | 0.2417 % 60.417 |
), ArticleFig(id=1154353353606816732, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789900721057930, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
| 进样量 | _告依春 | 芒果苷 | /连翘酯苷 I | / 连翘酯苷 A | / 松脂素吡喃葡糖糖苷 | /连翘酯素 |
| 5 | 3.1232 | 2.0503 | 1.7351 | 0.8689 | 0.9664 | 1.2909 |
| 10 | 3.1352 | 2.0841 | 1.7563 | 0.8728 | 0.9804 | 1.2978 |
| 15 | 3.1578 | 2.0927 | 1.7349 | 0.8821 | 0.9735 | 1.3002 |
| 20 | 3.1479 | 2.0678 | 1.7466 | 0.8735 | 0.9834 | 1.3147 |
| 25 | 3.1583 | 2.0591 | 1.7621 | 0.8804 | 0.9609 | 1.3185 |
| 30 | 3.1692 | 2.0866 | 1.7206 | 0.8651 | 0.9824 | 1.3212 |
| 平均值 | 3.1486 | 2.0734 | 1.7426 | 0.8738 | 0.9745 | 1.3072 |
| RSD/% | 0.54 | 0.82 | 0.88 | 0.75 | 0.94 | 0.96 |
), ArticleFig(id=1154353353678119902, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789900721057930, language=CN, label=表 2, caption=
各组分的相对校正因子, figureFileSmall=null, figureFileBig=null, tableContent=
| 进样量 | _告依春 | 芒果苷 | /连翘酯苷 I | / 连翘酯苷 A | / 松脂素吡喃葡糖糖苷 | /连翘酯素 |
| 5 | 3.1232 | 2.0503 | 1.7351 | 0.8689 | 0.9664 | 1.2909 |
| 10 | 3.1352 | 2.0841 | 1.7563 | 0.8728 | 0.9804 | 1.2978 |
| 15 | 3.1578 | 2.0927 | 1.7349 | 0.8821 | 0.9735 | 1.3002 |
| 20 | 3.1479 | 2.0678 | 1.7466 | 0.8735 | 0.9834 | 1.3147 |
| 25 | 3.1583 | 2.0591 | 1.7621 | 0.8804 | 0.9609 | 1.3185 |
| 30 | 3.1692 | 2.0866 | 1.7206 | 0.8651 | 0.9824 | 1.3212 |
| 平均值 | 3.1486 | 2.0734 | 1.7426 | 0.8738 | 0.9745 | 1.3072 |
| RSD/% | 0.54 | 0.82 | 0.88 | 0.75 | 0.94 | 0.96 |
), ArticleFig(id=1154353353762005985, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789900721057930, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
| 仪器 | 色谱柱 | |
| 芒果苷 /s | 连翘酯苷 I/s | 连翘酯苷 A/s | 松脂素吡喃葡糖糖苷 /s | 连翘酯素 |
| 安捷伦 1260 | Agilent 5 TC-C C18 | 0.2681 | 0.4496 | 0.6200 | 0.6928 | 0.7444 | 1.268 |
| YMC Hydrosphere C18 | 0.2709 | 0.4569 | 0.6283 | 0.6924 | 0.7514 | 1.2753 |
| Shimadzu AcclaimTM120 C18 | 0.2596 | 0.4474 | 0.6167 | 0.6831 | 0.7468 | 1.2513 |
| Agilent 5 TC-C C18 | 0.2608 | 0.4469 | 0.6164 | 0.6829 | 0.7613 | 1.2512 |
| 岛津 LC-2030C 3D Plus | YMC Hydrosphere C18 | 0.2633 | 0.4484 | 0.6178 | 0.6849 | 0.7466 | 1.2498 |
| Shimadzu AcclaimTM120 C18 | 0.2706 | 0.4567 | 0.6281 | 0.6922 | 0.7539 | 1.2757 |
| 平均值 | | 0.2656 | 0.4510 | 0.6212 | 0.6881 | 0.7507 | 1.2619 |
| RSD/% | | 1.9 | 1.0 | 0.89 | 0.71 | 0.83 | 0.99 |
), ArticleFig(id=1154353353824920546, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789900721057930, language=CN, label=表 3, caption=
各成分相对保留值, figureFileSmall=null, figureFileBig=null, tableContent=
| 仪器 | 色谱柱 | |
| 芒果苷 /s | 连翘酯苷 I/s | 连翘酯苷 A/s | 松脂素吡喃葡糖糖苷 /s | 连翘酯素 |
| 安捷伦 1260 | Agilent 5 TC-C C18 | 0.2681 | 0.4496 | 0.6200 | 0.6928 | 0.7444 | 1.268 |
| YMC Hydrosphere C18 | 0.2709 | 0.4569 | 0.6283 | 0.6924 | 0.7514 | 1.2753 |
| Shimadzu AcclaimTM120 C18 | 0.2596 | 0.4474 | 0.6167 | 0.6831 | 0.7468 | 1.2513 |
| Agilent 5 TC-C C18 | 0.2608 | 0.4469 | 0.6164 | 0.6829 | 0.7613 | 1.2512 |
| 岛津 LC-2030C 3D Plus | YMC Hydrosphere C18 | 0.2633 | 0.4484 | 0.6178 | 0.6849 | 0.7466 | 1.2498 |
| Shimadzu AcclaimTM120 C18 | 0.2706 | 0.4567 | 0.6281 | 0.6922 | 0.7539 | 1.2757 |
| 平均值 | | 0.2656 | 0.4510 | 0.6212 | 0.6881 | 0.7507 | 1.2619 |
| RSD/% | | 1.9 | 1.0 | 0.89 | 0.71 | 0.83 | 0.99 |
), ArticleFig(id=1154353353887835109, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789900721057930, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
| 批号 | 连翘苷/ (μg/mL) | (R, S)- 告依春 / (μg/mL) | 芒果苷/ | 连翘酯苷 | | 连翘酯苷A/(μg/mL) | 松脂素吡喃 葡糖糖苷/(μg/mL) | 连翘酯素/ (μg/mL) |
| ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM |
| S1 | 95.07 | 24.37 | 24.85 | 52.43 | 52.71 | 46.53 | 46.99 | 679.89 | 680.33 | 23.17 | 23.46 | 5.87 | 5.95 |
| S2 | 89.82 | 21.42 | 21.90 | 55.27 | 54.63 | 66.76 | 66.62 | 577.34 | 576.27 | 28.32 | 27.96 | 5.55 | 5.48 |
| S3 | 88.74 | 37.34 | 36.08 | 50.38 | 49.59 | 65.81 | 65.16 | 598.47 | 599.25 | 27.64 | 27.31 | 4.79 | 4.83 |
| S4 | 106.42 | 19.88 | 19.16 | 10.26 | 9.70 | 103.97 | 104.50 | 688.62 | 688.03 | 26.08 | 25.16 | 4.53 | 4.44 |
| S5 | 111.49 | 20.66 | 20.95 | 19.07 | 18.32 | 98.32 | 98.08 | 657.91 | 657.26 | 25.83 | 26.45 | 3.39 | 3.28 |
| S6 | 122.09 | 10.46 | 10.39 | 15.09 | 14.54 | 20.64 | 20.86 | 757.15 | 756.24 | 12.33 | 12.85 | 5.48 | 5.11 |
| S7 | 120.64 | 26.08 | 25.36 | 12.74 | 12.51 | 21.38 | 21.32 | 532.44 | 533.19 | 11.79 | 11.90 | 10.27 | 10.51 |
| S8 | 93.97 | 18.15 | 17.54 | 7.85 | 7.78 | 81.06 | 80.38 | 517.27 | 517.71 | 20.16 | 20.70 | 13.64 | 13.96 |
| S9 | 125.11 | 21.33 | 20.80 | 13.61 | 13.82 | 100.54 | 100.63 | 693.29 | 694.62 | 28.52 | 28.08 | 7.61 | 7.55 |
| S10 | 87.73 | 17.45 | 17.33 | 10.28 | 10.06 | 82.41 | 82.68 | 566.94 | 567.39 | 20.44 | 20.83 | 2.58 | 2.63 |
), ArticleFig(id=1154353353954943975, tenantId=1146029695717560320, journalId=1146119944283992078, articleId=1149789900721057930, language=CN, label=表 4, caption=
一测多评法和外标法测定结果, figureFileSmall=null, figureFileBig=null, tableContent=
| 批号 | 连翘苷/ (μg/mL) | (R, S)- 告依春 / (μg/mL) | 芒果苷/ | 连翘酯苷 | | 连翘酯苷A/(μg/mL) | 松脂素吡喃 葡糖糖苷/(μg/mL) | 连翘酯素/ (μg/mL) |
| ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM | QAMS | ESM |
| S1 | 95.07 | 24.37 | 24.85 | 52.43 | 52.71 | 46.53 | 46.99 | 679.89 | 680.33 | 23.17 | 23.46 | 5.87 | 5.95 |
| S2 | 89.82 | 21.42 | 21.90 | 55.27 | 54.63 | 66.76 | 66.62 | 577.34 | 576.27 | 28.32 | 27.96 | 5.55 | 5.48 |
| S3 | 88.74 | 37.34 | 36.08 | 50.38 | 49.59 | 65.81 | 65.16 | 598.47 | 599.25 | 27.64 | 27.31 | 4.79 | 4.83 |
| S4 | 106.42 | 19.88 | 19.16 | 10.26 | 9.70 | 103.97 | 104.50 | 688.62 | 688.03 | 26.08 | 25.16 | 4.53 | 4.44 |
| S5 | 111.49 | 20.66 | 20.95 | 19.07 | 18.32 | 98.32 | 98.08 | 657.91 | 657.26 | 25.83 | 26.45 | 3.39 | 3.28 |
| S6 | 122.09 | 10.46 | 10.39 | 15.09 | 14.54 | 20.64 | 20.86 | 757.15 | 756.24 | 12.33 | 12.85 | 5.48 | 5.11 |
| S7 | 120.64 | 26.08 | 25.36 | 12.74 | 12.51 | 21.38 | 21.32 | 532.44 | 533.19 | 11.79 | 11.90 | 10.27 | 10.51 |
| S8 | 93.97 | 18.15 | 17.54 | 7.85 | 7.78 | 81.06 | 80.38 | 517.27 | 517.71 | 20.16 | 20.70 | 13.64 | 13.96 |
| S9 | 125.11 | 21.33 | 20.80 | 13.61 | 13.82 | 100.54 | 100.63 | 693.29 | 694.62 | 28.52 | 28.08 | 7.61 | 7.55 |
| S10 | 87.73 | 17.45 | 17.33 | 10.28 | 10.06 | 82.41 | 82.68 | 566.94 | 567.39 | 20.44 | 20.83 | 2.58 | 2.63 |
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