UPLC-MS/MS法同时测定垂盆草总黄酮中8种成分的含量
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篇名: UPLC-MS/MS法同时测定垂盆草总黄酮中8种成分的含量
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摘要: 目的:建立同时测定垂盆草总黄酮中金丝桃苷、槲皮苷、木犀草苷、山柰酚、槲皮素、芦丁、木犀草素、异鼠李素含量的方法。方法:采用超高效液相色谱-串联质谱法。色谱柱为ZOBAX SB C18,流动相为甲醇-5 mmol/L甲酸铵水溶液(45 ∶ 55,V/V),流速为0.4 mL/min,柱温为30 ℃,进样量为2 μL;离子化模式为电喷雾电离,离子源温度为400 ℃,脱溶剂温度为300 ℃,脱溶剂流速为600 L/h,毛细管电压为3 000 V,雾化气压力为45 psi,工作模式为多反应监测模式,检测方式为负离子模式。采用建立的方法测定3批垂盆草总黄酮中8种成分的含量。结果:金丝桃苷、槲皮苷、木犀草苷、山柰酚、槲皮素、芦丁、木犀草素、异鼠李素检测质量浓度线性范围分别为10.0~640.0、0.5~32.0、4.5~288.0、8.0~512.0、50.0~3 200.0、2.0~128.0、12.5~800.0、25.2~1 612.8 ng/mL(r≥0.991 4),检测限分别为5.0、0.25、2.25、4.0、25.0、1.0、6.25、12.6 ng/mL,定量限分别为10.0、0.5、4.5、8.0、50.0、2.0、12.5、25.2    ng/mL;精密度、稳定性(24 h)、重复性试验的RSD均≤4.3%(n=6),加样回收率为95.9%~100.6%,RSD为1.5%~3.8%(n=6)。3批垂盆草总黄酮中金丝桃苷、槲皮苷、木犀草苷、山柰酚、槲皮素、芦丁、木犀草素、异鼠李素的含量分别为507.88~560.37、42.95~50.36、63.52~71.80、1 695.10~1 753.27、10 569.28~10 612.99、25.76~30.13、2 795.22~2 877.43、4 869.55~4 971.30 μg/g。结论:建立的方法可用于垂盆草总黄酮中8种成分含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of hyperoside, quercitrin, luteoloside, kaempferol, quercetin, rutin, luteolin and isorhamnetin in total flavanones of Sedum sarmentosum Bunge. METHODS: UPLC-MS/MS method was adopted. The determination was performed on ZOBAX SB C18 column with mobile phase consisted of methanol-5 mmol/L ammonium formate aqueous solution (45 ∶ 55, V/V) at the flow rate of 0.4 mL/min. The column temperature was 30 ℃, and sample size was 2 μL. The electrospray ionization source (ESI) was used; ion source temperature was 400 ℃; desolvation temperature was 300 ℃; desolvation gas flow was 600 L/h; capillary voltage was 3 000 V; nebuliser pressure was 45 psi; the work mode was multiple reaction monitoring mode; detection mode was negative ion mode. The established method was used to determine the contents of 8 components in 3 batches of total flavanones of Sedum sarmentosum Bunge. RESULTS: The linear ranges of hyperoside, quercitrin, luteoloside, kaempferol, quercetin, rutin, luteolin and isorhamnetin were 10.0-640.0, 0.5-32.0, 4.5-288.0, 8.0-512.0, 50.0-3 200.0, 2.0-128.0, 12.5-800.0 and 25.2-1 612.8 ng/mL (r≥0.991 4), respectively. The limits of detection were 5.0, 0.25, 2.25, 4.0, 25.0, 1.0, 6.25 and 12.6 ng/mL, respectively. The limits of quantitation were 10.0, 0.5, 4.5, 8.0, 50.0, 2.0, 12.5 and 25.2 ng/mL, separately. RSDs of precision, stability (24 h) and reproducibility tests were no more than 4.3% (n=6). The recoveries were 95.9%-100.6%, and RSDs were 1.5%-3.8% (n=6). The contents of hyperoside, quercitrin, luteoloside, kaempferol, quercetin, rutin, luteolin and isorhamnetin in 3 batches of total flavanones of Sedum sarmentosum Bunge were 507.88-560.37, 42.95-50.36, 63.52-71.80, 1 695.10-1 753.27, 10 569.28-10 612.99, 25.76-30.13, 2 795.22-2 877.43 and     4 869.55-4 971.30 μg/g, respectively. CONCLUSIONS: The established method can be used for simultaneous determination of 8 components in total flavanones of Sedum sarmentosum Bunge.
期刊: 2018年第29卷第9期
作者: 王雪,蒋志涛,严国俊,邵珠莹,冯星月,潘金火
AUTHORS: WANG Xue,JIANG Zhitao,YAN Guojun,SHAO Zhuying,FENG Xingyue,PAN Jinhuo
关键字: 垂盆草;总黄酮;超高效液相色谱-串联质谱法;含量测定
KEYWORDS: Sedum sarmentosum Bunge; Total flavanones; UPLC-MS/MS; Content determination
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