论文部分内容阅读
目的建立测定大鼠血浆及粪便中新疆紫草3种萘醌类成分含量的高效液相色谱法(HPLC法)。方法采用COSMOIL C_(18)-AR-Ⅱ(4.6mm×250mm,5μm)色谱柱,流动相A乙腈(A)-0.15%甲酸(B)(v/v)溶液,进行洗脱,流速1.0mL/min,检测波长275nm,柱温25℃,检测时间35min。结果血浆中左旋紫草素在0.40~6.40μg、乙酰紫草素在25.0~600.0μg、β,β′-二甲基丙烯酰紫草素在25.0~600.0μg范围内均与峰面积呈线性关系,左旋紫草素回收率为97.78%~100.1%、乙酰紫草素为100.1%~100.2%、β-β′-二甲基丙烯酰紫草素为97.78%~100.1%,日间、日内RSD均<1.5%。粪便中各组分在10~400μg/mL范围内与峰面积呈线性关系,平均回收率分别为(78.2±2.5)%、(82.0±2.9)%和(79.5±3.5)%。0~12、12~24、24~48h粪便中左旋紫草素绝对回收量分别为23.61、38.28、4.13mg;乙酰紫草素分别为7.20、70.78、11.53mg;β-β′二甲基丙烯酰紫草素分别为46.32、60.15、16.88mg。结论 HPLC法准确可靠,重复性好,适用于测定血浆及粪便中新疆紫草萘醌类成分含量。
OBJECTIVE To establish a high performance liquid chromatography (HPLC) method for the determination of three naphthoquinones in Lithospermum japonicus in plasma and feces of rats. Methods A mobile phase of acetonitrile (A) - 0.15% formic acid (B) (v / v) was eluted with COSMOIL C 18-18AR-Ⅱ (4.6 mm × 250 mm, / min, detection wavelength 275nm, column temperature 25 ℃, detection time 35min. Results In the range of 0.40-6.40μg of L-shikonin and 25.0-600.0μg of acetylshikonin in plasma, the peak area was linear with the range of 25.0-600.0μg , The recoveries of L-shikonin were 97.78% -100.1%, acetyl shikonin was 100.1% -100.2%, β-β’-dimethacryl shikonin was 97.78% -100.1%, intraday and intraday RSD All <1.5%. The excretion of each component in the range of 10 ~ 400μg / mL and the peak area was a linear relationship, the average recovery was (78.2 ± 2.5)%, (82.0 ± 2.9)% and (79.5 ± 3.5)%. The absolute recoveries of L-shikonin in feces of 0-12, 12-24, 24-48 hours were 23.61, 38.28, and 4.13 mg, respectively, while that of acetylshikonin was 7.20, 70.78 and 11.53 mg respectively. Β-β’-dimethylpropylene Acyl shikonin were 46.32,60.15,16.88mg. Conclusion The HPLC method is accurate and reproducible and has good reproducibility. It is suitable for the determination of naphthoquinones in Xinjiang and Xinjiang in plasma and excrement.