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作 者:孙艳涛[1,2] 宋玉红[1,2] 赵磊[3] 于浪天[4] 王良
机构地区:[1]吉林师范大学化学学院,吉林四平136000 [2]吉林师范大学环境友好材料制备与应用省部共建教育部重点实验室,吉林四平130103 [3]吉林省四平市食品药品检验所,吉林四平136099 [4]中国药科大学中药学院,南京211198
出 处:《中国药房》2017年第27期3862-3864,共3页China Pharmacy
摘 要:目的:建立同时测定牛黄宁宫片中6种成分含量的方法。方法:采用高效液相色谱法。色谱柱为TC-C_(18),流动相为甲醇-0.05%磷酸(梯度洗脱),流速为1.0 m L/min,检测波长为280 nm,柱温为25℃,进样量为10μL。结果:甘草苷、盐酸小檗碱、连翘苷、黄芩苷、大黄素和大黄酚检测质量浓度线性范围分别为3.2~320μg/m L(r=0.999 9)、8.8~880μg/m L(r=0.999 8)、5.6~560μg/m L(r=0.999 5)、2.0~200μg/m L(r=0.999 9)、4.4~440μg/m L(r=0.999 9)、2.0~200μg/m L(r=0.999 7);精密度、稳定性、重复性试验的RSD<6.0%;加样回收率分别为96.34%~97.25%(RSD=0.33%,n=6)、96.12%~98.06%(RSD=0.82%,n=6)、96.36%~99.09%(RSD=1.02%,n=6)、95.84%~97.32%(RSD=0.65%,n=6)、95.83%~97.92%(RSD=0.88%,n=6)、98.60%~99.65%(RSD=0.42%,n=6)。结论:该方法操作简便,精密度、稳定性、重复性好,可用于牛黄宁宫片中6种成分含量的测定。OBJECTIVE: To establish a method for simultaneous determination of 6 components in Niuhuang ninggong tablets. METHODS: HPLC method was adopted. The determination was performed on TC-C18 column with mobile phase consisted of meth- anol-0.05% phosphate acid (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 280 nm, and the column temperature was 25℃. The sample size was 10 μL. RESULTS: The linear ranges of glycyrrhizin, berberine hydrochloride, baicalin, baicalin, emodin and chrysophanol were 3.2-320 μg/mL(r=0.999 9), 8.8-880 μg/mL(r=0.999 8), 5.6-560 μg/mL (r= 0.999 5), 2.0-200 μg/mL(r=0.999 9), 4.4-440 μg/mL (r=0.999 9), 2.0-200 μg/mL(r=0.999 7), respectively. RSDs of preci- sion, stability and reproducibility tests were all lower than 6.0%. The recoveries were 96.34% -97.25% (RSD-0.33% , n=6), 96.12% -98.06% (RSD=0.82% , n=6) , 96.36% -99.09% (RSD=l.02% , n=6) , 95.84% -97.32% (RSD=0.65% , n=6) , 95.83%-97.92%(RSD=0.88% ,n=6), 98.60%-99.65%(RSD=0.42% ,n=6), respectively. CONCLUSIONS: The method is sim- ple, accurate, stable and reproducible, and can be used for content determination of 6 components in Niuhuang ninggong tablets.
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