摘要
建立苦木注射液总生物碱及单体有效成分苦木酮的含量测定方法,为该品种质量控制提供可靠的技术手段.根据苦木生物碱类成分的紫外-可见吸收光谱特征,选择以苦木酮为对照,300 nm为测定波长,直接光度法测定苦木注射液中总生物碱含量,线性范围为5~25μg/mL;反相高效液相色谱法测定苦木酮含量,在30℃柱温下,以乙腈-水(含0.1%乙酸)26∶74为流动相进行等度洗脱,检测波长为254 nm,苦木酮在5~30μg/mL浓度范围内与色谱峰面积呈良好线性关系(y=51.83x-60.11,r=0.999 8).系统的方法验证结果表明,所建立的2个含量测定方法专属性、精密度、准确度和耐用性良好,均符合药品质量标准的要求,适用于本品的质量控制;测得有效期内苦木注射液的总生物碱含量以苦木酮计平均为280μg/mL(RSD 7.0%,n=12),苦木酮含量平均为13.8μg/mL(RSD16.3%,n=20).
The methods for quantitation of total alkaloids and nigakinone, one of the main representative active alkaloid components in Kumu injection are established for its quality assessment and control. According to the UV- Vis spectroscopic characteristics of quassiawood alkaloids, the total alkaloids are determined by directly detecting the absorbance at 300 nm using nigakinone as a control, which provides a linear range of 5 -25 μg/mL. Nigaki- none is quantitated by a reversed-phase high performance liquid chromatographic method （RP-HPLC）. The mixture of acetonitrile and water （ containing 0. 1% acetic acid） at a volume ratio of 26 to 74 is applied for isocratic elution at a flow rate of 1 mL/min under a column temperature at 30 ℃. The detection wavelength is set at 254 nm, and good linearity between the chromatographic peak area of nigakinone and its concentration ranging from 5 to 30 μg/ mL is found with a typical regression equation of y = 51.83x - 60. 11 （ r = 0. 999 8 ）. Then method validation is performed to investigate specificity, precision, accuracy, and robustness, and the results indicates that both methods qualifiy for the quality control of Kumu injection. Several batches of products within shelf life are determined using the presently developed methods, and it is shown that that total alkaloids content calculated as nigakinone averages 280 μg/mL （ RSD 7.0% ,n = 12）, and nigakinone content 13.8 txg/mL （ RSD 16.3% ,n =20） in Kumu injection.
出处
《烟台大学学报（自然科学与工程版）》
CAS
2018年第1期32-37,共6页
Journal of Yantai University(Natural Science and Engineering Edition)
基金
烟台大学横向合作项目(HY15H35)
烟台大学实验室开放基金
烟台大学药学院实验室开放基金资助项目(烟台大学2016-2017年春、夏学期)
