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机构地区:[1]成都中医药大学药学院,成都611137 [2]成都市食品药品检验研究院,成都610000
出 处:《中国药房》2017年第36期5123-5126,共4页China Pharmacy
基 金:国家药品标准提高研究课题(No.2015-26)
摘 要:目的:建立同时测定腰痛胶囊中芍药苷、桂皮醛、补骨脂素、异补骨脂素含量的方法。方法:采用高效液相色谱法。色谱柱为Agilent-C18,流动相为乙腈-水(梯度洗脱),流速为1.0 mL/min,检测波长为240 nm(芍药苷、补骨脂素、异补骨脂素)、290 nm(桂皮醛),柱温为35℃,进样量为10μL。结果:芍药苷、桂皮醛、补骨脂素、异补骨脂素检测质量浓度线性范围分别为0.004 02~0.100 6 mg/mL(r=0.999 8)、0.024 50~0.612 7 mg/mL(r=0.999 8)、0.005 24~0.131 0 mg/mL(r=0.999 9)、0.005 11~0.127 8mg/mL(r=0.999 9);定量限分别为37.17、1.47、21.76、25.57 ng,检测限分别为11.15、0.44、6.53、7.67 ng;精密度、稳定性、重复性试验的RSD<2.0%;加样回收率分别为99.02%~100.83%(RSD=0.68%,n=6)、98.58%~100.99%(RSD=0.83%,n=6)、99.78%~101.69%(RSD=0.89%,n=6)、100.06%~102.46%(RSD=0.92%,n=6)。结论:该方法操作简单、结果准确,适用于腰痛胶囊中芍药苷、桂皮醛、补骨脂素、异补骨脂素含量的同时测定。OBJECTIVE: To establish a method for the simultaneous determination of paeoniflorin, cinnamaldehyde, psoralen and isopsoralen in Yaotong capsules. METHODS : HPLC method was adopted. The determination was performed on Agilent-C18 col- umn with mobile phase consisted of acetonitrile-water (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelengths were set at 240 nm (paeoniflorin, psoralen, isopsoralen) and 290 nm (cinnamaldehyde). The column temperature was 35 ℃, and sample size was 10 μL. RESULTS: The linear ranges of paeoniflorin, cirmamaldehyde, psoralen and isopsoralen were 0.004 02- 0.100 6 mg/mL(r=0.999 8), 0.024 50-0.612 7 mg/mL(r=0.999 8),0.005 24-0.131 0 mg/mL(r=0.999 9),0.005 11-0.127 8 mg/mL(r=0.999 9), respectively. LOQ were 37.17, 1.47, 21.76, 25.57 ng, respectively; LOD were 11.15, 0.44, 6.53, 7.67 ng, respectively. RSDs of precision, stability and reproducibility tests were all lower than 2.0%. The recoveries were 99.02%-100.83% (RSD=0.68%, n=6), 98.58% -100.99% (RSD=0.83%, n=6), 99.78% -101.69% (RSD=0.89%, n=6), 100.06% -102.46% (RSD=0.92%, n=6), respectively. CONCLUSIONS: The method is simple, accurate and suitable for simultaneous determination of paeoniflorin, cinnamaldehyde, psoralen and isopsoralen in Yaotong capsules.
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