UPLC-MS/MS法同时测定苦黄注射液中7种成分的含量
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篇名: UPLC-MS/MS法同时测定苦黄注射液中7种成分的含量
TITLE:
摘要: 目的:建立同时测定苦黄注射液中苦参碱、槐果碱、大黄素、大黄酸、绿原酸、柴胡皂苷a、芦荟大黄素含量的方法。方法:采用超高效液相色谱-串联质谱法。色谱柱为 Phenomenex Kinetex C18,流动相为甲醇-0.1%甲酸(梯度洗脱),流速为0.5 mL/min,柱温为20 ℃,进样器温度为10 ℃,平衡时间为4 min,进样量为5  μL。离子化模式为电喷雾电离,源喷射电压分别为5 500、-4 500 V,雾化气压力为4.14×105 Pa,加热气压力为4.48×105 Pa,帘气压力为1.72×105 Pa,离子源温度为600 ℃,工作模式为多反应监测模式。结果:苦参碱、槐果碱、大黄素、大黄酸、绿原酸、柴胡皂苷a、芦荟大黄素检测质量浓度线性范围分别为1.25~80.0 ng/mL(r=0.999 3)、1.10~70.0  ng/mL(r=0.999 5)、0.16~10.5  ng/mL(r=0.999 3)、2.61~168 ng/mL(r=0.999 3)、1.50~96.0  ng/mL(r=0.999 3)、1.48~94.5  ng/mL(r=0.999 6)、6.11~391 ng/mL(r=0.999 1);定量限分别为0.061、0.109、0.041、1.313、0.500、0.492、3.055 ng/mL,检测限分别为0.025、0.054、0.016、0.656、0.150、0.148、1.528 ng/mL;精密度、稳定性、重复性试验的RSD≤3%;加样回收率分别为95.45%~99.45%(RSD=1.43%,n=6)、97.50%~101.00%(RSD=1.50%,n=6)、95.67%~101.73%(RSD=2.85%,n=6)、97.17%~100.57%(RSD=1.16%,n=6)、95.19%~98.90%(RSD=1.71%,n=6)、95.38%~103.85%(RSD=3.39%,n=6)、95.50%~101.17%(RSD=1.20%,n=6)。结论:该方法简便、高效、准确、可靠,适用于同时测定苦黄注射液中7种有效成分的含量。
ABSTRACT: OBJECTIVE: To establish a method for the content determination of matrine, sophocarpine, emodin, rhein, chlorogenic acid, sarkosaponin a, aloe-emodin in Kuhuang injection.METHODS: UPLC-MS/MS was adopted. The determination was performed on Phenomenex Kenetix C18 column with mobile phase consisted of methanol-0.1% formic acid (gradient elution) at the flow rate of 0.5 mL/min. The column temperature was set at 20 ℃, and injector temperature was set at 10 ℃. The equilibrium time was 4 min and sample size was 5 μL. Ionization mode was electrospray ionization with spray voltage of 5 500 V and -4 500 V, atomizing air pressure of 4.14×105 Pa, heater pressure of 4.48×105 Pa, curtain air of 1.72×105 Pa and ion source temperature of 600 ℃. The work mode was multiple reaction monitoring mode. RESULTS: The linear range were 1.25-80.0 ng/mL for matrine (r=0.999 3),1.10-70.0 ng/mL for sophocarpine (r=0.999 5), 0.16-10.5 ng/mL for emodin (r=0.999 3), 2.61-168 ng/mL for rhein (r=0.999 3), 1.50-96.0 ng/mL for chlorogenic acid (r=0.999 3),1.48-94.5 ng/mL for sarkosaponin a (r=0.999 6) and 6.11-391 ng/mL for aloe-emodin (r=0.999 1). The limits of quantification were 0.061,0.109,0.041,1.313,0.500,0.492,3.055 ng/mL,limits of detection were 0.025,0.054,0.016,0.656,0.150,0.148,1.528 ng/mL. RSDs of precision, stability and reproducibility tests were all no more than 3%. The recoveries of them were 95.45%-99.45%(RSD=1.43%,n=6), 97.50%-101.00%(RSD=1.50%,n=6), 95.67%-101.73%(RSD=2.85%,n=6), 97.17%-100.57% (RSD=1.16%,n=6),95.19%-98.90%(RSD=1.71%,n=6), 95.38%-103.85%(RSD=3.39%,n=6), 95.50%-101.17%(RSD=1.20%,n=6), respectively. CONCLUSIONS: The method is simple, effective, accurate, reliable and suitable for simultaneous determination for 7 components in Kuhuang injection.
期刊: 2017年第28卷第15期
作者: 李宵,吴茵,支旭然,李倩,李颖,董占军
AUTHORS: LI Xiao,WU Yin,ZHI Xuran,LI Qian,LI Ying,DONG Zhanjun
关键字: 苦黄注射液;超高效液相色谱-串联质谱法;苦参碱;槐果碱;大黄素;大黄酸;绿原酸;柴胡皂苷a;芦荟大黄素
KEYWORDS: Kuhuang injection; UPLC-MS/MS; Matrine; Sophocarpine; Emodin; Rhein; Chlorogenic acid; Sarkosaponin a; Aloe-emodin
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