UPLC-MS/MS法同时测定裸花紫珠干浸膏中5 种有效成分的含量
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篇名: UPLC-MS/MS法同时测定裸花紫珠干浸膏中5 种有效成分的含量
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摘要: 目的: 建立同时测定裸花紫珠干浸膏中5 种有效成分含量的方法。方法:采用超高效液相色谱-串联质谱法。色谱条件:色谱柱为Zorbax Eclipse Plus C18,流动相为乙腈-水(梯度洗脱),流速为0.3 mL/min,柱温为40 ℃,进样量为2 μL;质谱条件:多反应监测离子扫描模式,干燥气/雾化气为氮气,干燥气温度为325 ℃,干燥气流量为6 L/min,雾化气压力为45 psi,鞘流气温度为350 ℃,鞘流气流量为12 L/min,毛细管电压为4 000 V(+)、3 500 V(-),喷嘴电压为500 V。结果:木犀草苷、毛蕊花糖苷、槲皮素、木犀草素、芦丁检测质量浓度线性范围分别为0.504 8~252.4 ng/ mL(r=0.999 9)、0.712 4~356.2 ng/mL(r=0.999 0)、0.509 4~254.7 ng/mL(r=0.996 2)、0.303 0~151.5 ng/ mL(r=0.999 8)、0.602 2~301.1 ng/ mL(r=0.999 6);精密度、稳定性、重复性试验的RSD<3.0%;定量限分别为0.42、0.87、0.33、0.12、0.76 ng/mL;加样回收率分别为97.99%~101.20%(RSD=1.3%,n=6)、96.50%~101.20%(RSD=1.7%,n=6)、94.81%~99.34%(RSD=1.7%,n=6)、97.54%~100.51%(RSD=1.2%,n=6)、93.37%~98.70%(RSD=1.9%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于裸花紫珠干浸膏中5 种有效成分含量的同时测定。
ABSTRACT: OBJECTIVE: To establish a method for simultaneous determination of 5 effective components in Luohua zizhu dry extract. METHODS: UPLC-MS/MS was conducted. The separation was performed on an Zorbax Eclipse Plus C18 column with mobile phase of acetonitrile-water (gradient elution) at the flow rate of 0.3 mL/min. The column temperature was set at 40 ℃ and sample size was 2 μL. The analytes were detected in the multiple reaction monitoring (MRM) mode. Nitrogen was used as drying gas and atomized gas. The temperature and flow rate of drying gas were 325 ℃ and 6 L/min. The pressure of atomized gas was 45 psi. The temperature and flow rate of sheath gas were 350 ℃ and 12 L/min. The voltage of capillary were 4 000 V(+) and 3 500 V(-). The voltage of nozzle was 500 V. RESULTS:The linear ranges of luteoloside,acteoside,quercetin,luteolin and rutin were 0.504 8- 252.4 ng/mL(r=0.999 9),0.712 4-356.2 ng/mL(r=0.999 0),0.509 4-254.7 ng/mL(r=0.996 2),0.303 0-151.5 ng/mL(r=0.999 8) and 0.602 2-301.1 ng/mL (r=0.999 6), respectively. RSDs of precision, stability and reproducibility tests were all less than 3.0%. The limit of quantitation were 0.42,0.87,0.33,0.12,0.76 ng/mL. The recoveries were 97.99%-101.20% (RSD=1.3%,n=6), 96.50%-101.20% (RSD=1.7%,n=6), 94.81%-99.34% (RSD=1.7%,n=6), 97.54%-100.51% (RSD=1.2%,n=6),93.37%-98.70% (RSD=1.9%,n=6), respectively. CONCLUSIONS: The method is simple, precise, stable and reproducible, and can be used for simultaneous determination of 5 effective components in Luohua zizhu dry extract.
期刊: 2017年第28卷第21期
作者: 郑培,汤兵力,林艳珠,冯春艳,刑征宇
AUTHORS: ZHENG Pei,TANG Bingli,LIN Yanzhu,FENG Chunyan,XING Zhengyu
关键字: 超高效液相色谱-串联质谱法;裸花紫珠干浸膏;木犀草苷;毛蕊花糖苷;槲皮素;木犀草素; 芦丁
KEYWORDS: UPLC-MS/MS; Luohua zizhu dry extract; Luteoloside; Acteoside; Quercetin; Luteolin; Rutin
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