UPLC-MS/MS法测定黄杨宁制剂中的环维黄杨星D的含量
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摘要
目的:建立超高效液相色谱-串联质谱法(UPLC-MS/MS)快速测定黄杨宁制剂中环维黄杨星D的含量。方法:采用UPLC-MS/MS法。色谱柱为Waters ACQUITY UPLC BEH C_(18)柱(100 mm×2.1 mm,1.7μm),流动相为乙腈-含0.1%甲酸的0.01 mol·L~(-1)甲酸氨溶液,梯度洗脱,流速为0.35 ml·min~(-1),柱温为30℃,进样量为5μl。离子源为电喷雾(ESI)离子源,正离子模式,工作模式为多反应监测模式(MRM)。结果:环维黄杨星D的线性范围为15.58~1 558.00 ng·ml~(-1)(r=0.999 5);平均加样回收率为97.7%(RSD=3.8%,n=6)。结论:该方法快速、简便、准确、重复性好,适用于黄杨宁制剂的质量控制。
Objective: To establish a method for the determination of cyclovirobuxium D in Huangyangning pharmaceutical preparations by UPLC-MS/MS. Methods: UPLC-MS/MS was conducted. The column was Waters ACQUITY UPLC BEH C_(18) column( 100 mm × 2. 1 mm,1. 7 μm),the mobile phase consisted of acetonitrile and 0. 01 mol · L~(-1) ammonium formate solution( containing0. 1% formic acid) with gradient elution at a flow rate of 0. 35 ml· min~(-1). The column temperature was 30℃ and the injection volume was 5 μl. The ionization mode was electrospray ionization( ESI) with a positive mode. Cyclovirobuxium D was analyzed with a multiple-reaction monitoring mode( MRM). Results: The linear range of cyclovirobuxium D was 15. 58-1558. 00 ng · ml~(-1)( r =0. 999 5). The average recovery of cyclovirobuxium D was 97. 7%( RSD = 3. 8%,n = 6). Conclusion: The method is rapid,simple and accurate with good reproducibility. It is applicable in the determination of cyclovirobuxium D in Huangyangning pharmaceutical preparations to be beneficial to the quality control of Huangyangning pharmaceutical preparations.
Objective: To establish a method for the determination of cyclovirobuxium D in Huangyangning pharmaceutical preparations by UPLC-MS/MS. Methods: UPLC-MS/MS was conducted. The column was Waters ACQUITY UPLC BEH C_(18) column( 100 mm × 2. 1 mm,1. 7 μm),the mobile phase consisted of acetonitrile and 0. 01 mol · L~(-1) ammonium formate solution( containing0. 1% formic acid) with gradient elution at a flow rate of 0. 35 ml· min~(-1). The column temperature was 30℃ and the injection volume was 5 μl. The ionization mode was electrospray ionization( ESI) with a positive mode. Cyclovirobuxium D was analyzed with a multiple-reaction monitoring mode( MRM). Results: The linear range of cyclovirobuxium D was 15. 58-1558. 00 ng · ml~(-1)( r =0. 999 5). The average recovery of cyclovirobuxium D was 97. 7%( RSD = 3. 8%,n = 6). Conclusion: The method is rapid,simple and accurate with good reproducibility. It is applicable in the determination of cyclovirobuxium D in Huangyangning pharmaceutical preparations to be beneficial to the quality control of Huangyangning pharmaceutical preparations.
引文
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7 郭青,吕霞,孙珊,等.黄杨宁原料及片中环维黄杨星D含量及含量均匀度测定[J].药物分析杂志,2009,29(10):1651-1657
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9 谢昀,于治国,徐新盛,等.反相离子对色谱法测定环维黄杨星D[J].药物分析杂志,2006,26(7):888-890
10 陈勇,樊雪君,龚青.HPLC梯度洗脱法测定黄杨宁片中环维黄杨星D的含量[J].中国中药杂志,2006,31(14):1155-1156
11 吕霞,胡明通,杨春,等.HPLC-ELSD法测定黄杨宁片中环维黄杨星D的含量[J].现代中药研究与实践,2014,28(3):52-54
2 满红梅.黄杨宁片联合参松养心胶囊治疗室性早搏的动态心电图评价[J].世界最新医学信息文摘,2016,16(41):143-144
3 吴寅莹.黄杨宁联合酒石酸美托洛尔治疗室性期前收缩65例临床观察[J].齐齐哈尔医学院学报,2015,36(29):4427-4428
4 魏秀敏.黄杨宁治疗心律失常的临床应用效果观察[J].首都食品与医药,2015(16):71-72
5 国家食品药品监督管理局标准[S].YBZ10862009
6 徐新军,张正行,盛龙生,等.柱前荧光衍生化RP-HPLC测定环维黄杨星D含量[J].药学学报,2002,37(5):359-361
7 郭青,吕霞,孙珊,等.黄杨宁原料及片中环维黄杨星D含量及含量均匀度测定[J].药物分析杂志,2009,29(10):1651-1657
8 郭青,吕霞,伍乃英,等.黄杨宁片及原料中环维黄杨星D含量测定的3种HPLC方法评价[J].中国现代应用药学,2009,26(11):929-933
9 谢昀,于治国,徐新盛,等.反相离子对色谱法测定环维黄杨星D[J].药物分析杂志,2006,26(7):888-890
10 陈勇,樊雪君,龚青.HPLC梯度洗脱法测定黄杨宁片中环维黄杨星D的含量[J].中国中药杂志,2006,31(14):1155-1156
11 吕霞,胡明通,杨春,等.HPLC-ELSD法测定黄杨宁片中环维黄杨星D的含量[J].现代中药研究与实践,2014,28(3):52-54