HPLC法同时测定蟾龙定喘合剂中5种成分的含量

Simultaneous Determination of 5 Components in Chanlong Dingchuan Mixture by HPLC

目的：建立同时测定蟾龙定喘合剂中补骨脂素、异补骨脂素、朝藿定B、朝藿定C和淫羊藿苷含量的方法。方法：采用高效液相色谱法。色谱柱为WelchMaterialsC18,流动相为乙腈-甲醇（1：1，V／V）-水（梯度洗脱），流速为0．9ml／min，检测波长为246nm（补骨脂素和异补骨脂素）、270nm（朝藿定B、朝藿定C和淫羊藿苷），柱温为30℃，进样量为20μl。结果：补骨脂素、异补骨脂素、朝藿定B、朝藿定C和淫羊藿苷的检测质量浓度线性范围分别为8．24～164．80pg／ml（r=0．9997）、5．15～103．00gg／ml（r=0．9993）、4．06～81．20gg／ml（r=0．9996）、5．88～117．60gg／ml（r=0．9995）、4．90-98．00μg／ml（r=0．9998）；定量限分别为0．385、0．179、0．124、0．218、0．348μg／ml，检测限分别为0．127、0．059、0．041、0．072、0．115gg／ml；精密度、稳定性、重复性试验的RSD〈2．0％；加样回收率分别为97．93％～100．06％（RSD=0．80％，n=6）、96．91％～100．16％（RSD=1．37％，n=6）、96．95％～99．63％（RSD=0．98％，n=6）、96．69％～99．33％（RSD=1．03％，n=6）、96．76％～98．53％（RSD=0．70％，n=6）。结论：该方法操作简便、结果可靠，适用于同时测定蟾龙定喘合剂中补骨脂素、异补骨脂素、朝藿定B、朝藿定c和淫羊藿苷的含量。

OBJECTIVE： To establish a method for the simultaneous determination of psoralen, isopsoralen, epimedin B, epi- medin C and icariin in Chanlong dingchuan mixture. METHODS： HPLC was performed on the column of Welch Materials C18 with mobile phase of acetonitrile - methanol （1：1, F/V）-water （gradient elution） at a flow rate of 0.9 ml/min, the detection wavelength was 246 nm （psoralen, isopsoralen） and 270 nm （epimedin B, epimedin C and icariin）, column temperature was 30 ℃, injection volume was 20 91. RESULTS： The linear range was 8.24-164.80 μg/ml for psoralen （r=0.999 7）, 5.15-103.00 μg/ml for isopso- ralen （r=0.999 3）,4.06-81.20 μg/ml for epimedin B （r=0.999 6）, 5.88-117.60μg/ml for epimedin C（r=0.999 5） and 4.90-98.00 μg/ml for icariin （r=0.999 8）; the limits of quantitation were 0.385 pg/ml, 0.179 μg/ml , 0.124 μg/ml, 0.218μg/ml and 0.348 μg/ml, limits of detection were 0.127μg/ml, 0.059 μg/ml , 0.041 μg/ml, 0.072 μg/ml and 0.115 μg/ml; RSDs of precision, stability and reproducibility tests were lower than 2.0%; recoveries were 97.93%-100.06% （RSD=0.80%, n=6）, 96.91%-100.16% （RSD= 1.37%,n=6）, 96.95%-99.63% （RSD=0.98%,n=6）, 96.69%-99.33% （RSD=1.03%,n=6）and 96.76%-98.53% （RSD= 0.70%, n = 6）, respectively. CONCLUSIONS： The method is simple and reliable, and suitable for the simultaneous determination of psoralen, isopsoralen, epimedin B, epimedin C and icariin in Chanlong dingchuan mixture.