UPLC-MS/MS法测定大株红景天注射液中红景天苷和酪醇的含量
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摘要
目的建立一种UPLC-MS/MS法同时测定大株红景天注射液中红景天苷和酪醇的含量。方法色谱柱为XBridge~?BEH C_(18)(2. 1 mm×100. 0 mm,2. 5μm),流动相为乙腈-0. 05%甲酸水,梯度洗脱,流速为0. 3 mL·min~(-1),进样量为5μL,柱温为30℃;用电喷雾离子源进行负离子监测模式,多反应监测模式用于定量分析。考察该方法的专属性、标准曲线和定量下限、精密度与回收率、稳定性以及重现性。结果大株红景天注射液中的红景天苷和酪醇分别在12. 50～800. 00和54. 69～1750. 00 ng·mL~(-1)内,线性关系良好,定量下限分别为0. 31和6. 84 ng·mL~(-1),标准曲线分别为y=1. 24×10~4x+1. 42×10~4(r=0. 999 8)和y=1. 11×10~4x+8. 97×10~4(r=0. 999 9),精密度分别为0. 98%和1. 41%,平均加样回收率分别为97. 04%和96. 79%。5批样品中红景天苷和酪醇含量测定结果分别为3. 62～3. 87和2. 02～2. 13 mg·mL~(-1)。结论本方法快速准确灵敏、重复性好,可用于大株红景天注射液中红景天苷和酪醇的定量测定。
Objective To develop a method for the simultaneous determination of the salidroside and tyrosol in sofren injection by UPLC-MS/MS. Methods The samples were separated on a XBridge~? BEH C_(18)( 2. 1 mm × 100. 0 mm,2. 5 μm). The mobile phase was composed of acetonitrile and 0. 05% aqueous formic acid with gradient elution. The injection volume was 5 μL and the flow rate was 0. 3 mL·min~(-1). The column temperature was 30℃. Multiple-reaction monitoring scanning was employed for quantification with electrospray ion source polarity in negative ion. Results The validated method had excellent linearities in the range of 12. 50-800. 00 and 54. 69~(-1)750. 00 ng·mL~(-1) for salidroside and tyrosol in sofren injection,with the limits of quantification at0. 31 and 6. 84 ng·m L~(-1). The standard curves were y = 1. 24 × 10~4 x +1. 42 × 10~4( r =0. 999 8) and y = 1. 11 × 10~4 x + 8. 97 × 10~4( r = 0. 999 9),the precisions were 0. 98% and 1. 41%, respectively. The average recoveries of sample addition were 97. 04% and 96. 79%, and the contents in 5 samples were 3. 62-3. 87 and 2. 02-2. 13 mg · mL~(-1),respectively. Conclusion The method is rapid,accurate,sensitive and with good reproducibility and can be used for the determination of salidroside and tyrosol in sofren injection.
Objective To develop a method for the simultaneous determination of the salidroside and tyrosol in sofren injection by UPLC-MS/MS. Methods The samples were separated on a XBridge~? BEH C_(18)( 2. 1 mm × 100. 0 mm,2. 5 μm). The mobile phase was composed of acetonitrile and 0. 05% aqueous formic acid with gradient elution. The injection volume was 5 μL and the flow rate was 0. 3 mL·min~(-1). The column temperature was 30℃. Multiple-reaction monitoring scanning was employed for quantification with electrospray ion source polarity in negative ion. Results The validated method had excellent linearities in the range of 12. 50-800. 00 and 54. 69~(-1)750. 00 ng·mL~(-1) for salidroside and tyrosol in sofren injection,with the limits of quantification at0. 31 and 6. 84 ng·m L~(-1). The standard curves were y = 1. 24 × 10~4 x +1. 42 × 10~4( r =0. 999 8) and y = 1. 11 × 10~4 x + 8. 97 × 10~4( r = 0. 999 9),the precisions were 0. 98% and 1. 41%, respectively. The average recoveries of sample addition were 97. 04% and 96. 79%, and the contents in 5 samples were 3. 62-3. 87 and 2. 02-2. 13 mg · mL~(-1),respectively. Conclusion The method is rapid,accurate,sensitive and with good reproducibility and can be used for the determination of salidroside and tyrosol in sofren injection.
引文
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[2]王雪晶,谢雪,罗鑫,等.大株红景天化学成分研究(I)[J].中草药,2015,46(23):3471-3474.
[3]关潇滢,王铁杰,李军,等.HPLC法同时测定大株红景天中红景天苷、酪醇和没食子酸的含量[J].沈阳药科大学学报,2010,27(5):377-380.
[4]支旭然,王觅,宋浩静,等.UPLC-MS/MS法同时测定舒肝宁注射液中6个成分的含量[J].药物分析杂志,2018,38(12):2194-2199.
[5]吴趋凡,李耿,符崖.LC-MS/MS同时测定大鼠血浆中红景天苷和酪醇及其药物代谢动力学研究[J].中药新药与临床药理,2013,24(2):169-172.