论文部分内容阅读
目的:建立测定复方制剂中盐酸赖氨酸含量的方法。方法:采用邻苯二甲醛(OPA)柱前衍生化高效液相色谱法。色谱柱为Kromasil C18,流动相为0.04 mol/L磷酸二氢钠溶液(10%氢氧化钠溶液调节p H至7.2)-甲醇-乙腈(70∶15∶15,V/V/V),流速为1.5 ml/min,检测波长为338 nm,柱温为35℃,供试品与OPA衍生剂及硼酸盐缓冲液按设定程序自动混匀后进样。结果:盐酸赖氨酸质量浓度在0.027 4~0.438 8 mg/ml范围内与峰面积呈良好的线性关系(r=0.999 5);精密度、稳定性、重复性试验的RSD≤0.84%;在五维赖氨酸颗粒、赖氨肌醇维B12口服溶液、赖氨酸磷酸氢钙片中盐酸赖氨酸的平均加样回收率分别为99.8%(RSD=0.86%,n=9)、100.1%(RSD=0.79%,n=9)、99.6%(RSD=0.65%,n=9)。对3批含盐酸赖氨酸的复方制剂进行含量测定,所得结果与原质量标准测定方法中的结果一致。结论:该方法样品处理简单快速,可用于含有盐酸赖氨酸的复方制剂的质量控制。
Objective: To establish a method for determination of lysine hydrochloride in compound preparations. Methods: OPA column precolumn derivatization high performance liquid chromatography. The column was Kromasil C18 and the mobile phase consisted of 0.04 mol / L sodium dihydrogen phosphate solution (adjusted to pH 7.2 from 10% sodium hydroxide solution) -methanol-acetonitrile (70:15:15, V / V / V) 1.5 ml / min, the detection wavelength was 338 nm, the column temperature was 35 ℃, the sample and OPA derivatizing agent and borate buffer according to the set program automatically mix after injection. Results: The concentration of lysine hydrochloride showed a good linear relationship with the peak area in the range of 0.027 4-0.438 8 mg / ml (r = 0.999 5). The RSD of precision, stability and repeatability was ≤0.84% The average recoveries of five-dimensional lysine granules, lysostaphin B12 oral solution and lysine calcium phosphate tablets were 99.8% (RSD = 0.86%, n = 9), 100.1 % (RSD = 0.79%, n = 9), 99.6% (RSD = 0.65%, n = 9). The contents of three batches of compound preparation containing hydrochloric acid lysine were determined, and the results were consistent with the results of the original quality standard determination method. Conclusion: This method is simple and rapid sample processing, can be used for the quality control of the compound preparation containing lysine hydrochloride.