摘要
目的:建立热感赛比斯坦颗粒定性定量方法。方法:采用薄层色谱法对热感赛比斯坦颗粒中罂粟壳、罂粟子、甘草、破布木果、蜀葵子、黄瓜子、榅桲子和巴旦仁进行定性鉴别;采用高效液相色谱法测定热感赛比斯坦颗粒中甘草苷、甘草酸铵和吗啡的含量。甘草苷和甘草酸铵含量测定色谱条件:采用Agilent TC C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈(A)-0.1%磷酸溶液(B)为流动相,梯度洗脱(0-10 min,19%A;10-15 min,19%A→25%A;15-30 min,25%A→38%A;30-42 min,38%A;42-50 min,38%A→19%A),流速1 m L·min^-1,检测波长237 nm,柱温为30℃;吗啡含量测定色谱条件:采用Phenomenex Luna C8(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.5%醋酸铵水溶液(含三乙胺0.8%)(13∶87)为流动相,流速1.0 m L·min^-1,检测波长286 nm,柱温30℃。结果:TLC斑点清晰,分离度好,阴性无干扰。甘草苷、甘草酸铵和吗啡质量浓度分别在3.68-73.64、18.62-260.68和5.33-85.28μg·m L^-1范围内,与峰面积线性关系良好,r分别为0.999 8、0.999 9和0.999 8);平均回收率(n=6)分别为102.9%、102.2%和99.71%,RSD分别为0.98%、1.4%和1.7%。结论:所建方法可用于热感赛比斯坦颗粒的质量控制。
Objective: To establish the qualitative and quantitative methods of Regansaibisitan granules. Methods:Papaveris Pericarpium,Semen Papaveris,Glycyrrhizae Radix et Rhizoma,Fructus Cordiae Dichotomae,Semen Althaeae Roseae,Semen Cucumeris,Semen Cydoniae,Semen Amygdali Dulcis were identified by TLC. The contents of liquiritin,ammonium glycyrrhetate and morphine were determined by HPLC. The determination of liquiritin and ammonium glycyrrhetate was performed on Agilent TC C18( 250 mm × 4. 6 mm,5 μm); the mobile phase consisted of acetonitrile( A)-0. 1% phosphoric acid solution( B) with gradient elution [0-10 min,19% A; 10-15 min,19% A→25% A; 15-30 min,25% A→38% A; 30-42 min,38% A; 42-50 min,38% A→19% A]at the flow rate of 1 m L·min^-1; the column temperature was 30 ℃ and the detection wavelength was 286 nm. The determination of morphine was performed on the Phenomenex Luna C8( 250 mm × 4. 6 mm,5 μm) column; the mobile phase consisted of acetonitrile solution and 0. 5% ammonium acetate solution( containing 0. 8% triethylamine)( 13∶ 87)at the flow rate of 1. 0 m L·min^-1; the detection wavelength was 286 nm and the column temperature was 30 ℃.Results: TLC spots were clear and well-separated without interference from negative samples. The linear response ranges of liquiritin,ammonium glycyrrhetate and morphine were 3. 68-73. 64 μg·m L^-1,18. 62-260. 68 μg·m L^-1,and 5. 33-85. 28 μg·m L^-1,r = 0. 999 8,0. 999 9,0. 999 8,respectively. The average recoveries( n =6) were 102. 9%,102. 2%,99. 71% and RSDs were 0. 98%,1. 4%,1. 7%,respectively. Conclusion: The established method can be used for quality control of Regansaibisitan granules.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第1期139-145,共7页
Chinese Journal of Pharmaceutical Analysis
基金
自治区优秀青年科技创新人才培养项目(2013721034)
关键词
热感赛比斯坦颗粒
维药质量控制
罂粟壳
罂粟子
甘草
破布木果
蜀葵子
黄瓜子
榅桲子
巴旦仁
薄层色谱法
高效液相色谱法
Regansaibisitan granules
quality control of Uygur medicine
Papaveris Pericarpium
Semen Papaveris
Glycyrrhizae Radix et Rhizoma
Fructus Cordiae Dichotomae
Semen Althaeae Roseae
Semen Cucumeris
Semen Cydoniae
Semen Amygdali Dulcis
TLC
HPLC