香黄通便胶囊中木香烃内酯、去木香烃内酯含量测定的研究

The study of determination of Costunolide and Dehydrocostuslactone in Xianghuangtongbian Capsule

目的采用高效液相色谱法，对香黄通便胶囊中木香烃内酯、去木香烃内酯进行含量测定研究。方法①高效液相色谱法：检测木香烃内酯、去木香烃内酯的含量。参考文献选择合适的固定相，调整流动相组成、配比、流速以及柱温，在最大吸收波长下测定，使指标峰分离完全，理论塔板数符合要求。②线性范围考察：配制系列浓度的对照品溶液．以色谱峰的峰面积为纵坐标，以进样浓度为横坐标，进行线性回归，得回归曲线并考察线性范围。③方法学考察：分别考察测定方法的重复性、重现性、耐用性、稳定性和加样回收率。④样品含量测定：取三批样品分别按上述方法测定指标成分的含量。结果香黄通便胶囊中木香烃内酯、去木香烃内酯色谱条件为：AgilentZorbaxSB—C13色谱柱，流动相：甲醇-水（65：35，V/V），流速：0．8mL／min，柱温：25clC，检测波长：225nm。木香烃内酯、去木香烃内酯分别在14．4-216．0txg／mL、28．0-421．2μg／mL范围内线性关系良好，r分别为0．9996、0．9999。该方法重复性、重现性、耐用性、在12h内稳定性的RSD分别为0．77％、03晚，0．05％、0．59％，0．88％、1．30％，1．54％、0．43％。三个浓度（80％、100％、120％）的加样回收率为99．2％、102．9％，100．9％、101．8％，97．5％、100．5％，RSD分别为0．84％、0-31％，0．20％、1．70％，0．18％、0．12％。样品中木香烃内酯、去木香烃内酯总含量不低于4．22m∥粒。结论以木香烃内酯、去木香烃内酯作为含量测定指标，采用高效液相色谱法进行检测，准确度高，专属性强，重现性好。

Objective To measure the content of Costunolide and Dehydrocostus lactone in Xianghuangtongbian Cap- sule by using highly-effective liquid chromatography. Methods ①HPLC： The contents of Costunolide and Dehydrocos- tus laetone was detected separately. Proper stationary phase was chosed, the makeup, matching, flow rate and column temperature of mobile phase was adjusted, in the condition of wavelength （nm） max, the absorption peaks were separat- ed completely, the theoretical plate number meet the standard. ②Linearity range investigation： Reference substance so- lution of different concentration were confected, the linear regression was performed with chromatographic peak area as y-axis and sampling concentration as x-axis, the curvilinear regression was to get, and the linearity range was investi- gated. ③Methodological investigation： the repeatability, reproducibility, durability, stability and sample recovery rate of the method were investigated. ④Sample content determination： determining the content of index components in three groups of samples according to the methods mentioned above. Results The concentration of Costunolide and Dehydro- costus lactone in Xianghuangtongbian Capsule was determined using a HPLC system at the wavelength of 225 nm. The separation was achieved by using a Agilent Zorbax SB-C is, at a rate of 0.8 mL/min. The temperature of column was 25℃. The mobile phase consisted of methyl alcohol and water at a ratio of 65：35 （V/V）, Costunolide and Dehydroeostus laetone had a good linear relationship among 14.4-216.0 μg/mL, 28.0 - 421.2 ptg/mL, r was 0.9996 and 0.9999. TheRSD% of repeatability, reproducibility, durability, the stability within 12 hours and analytical recovery were 0.77%, 0.30%; 0.05%, 0.59%; 0.88%, 1.30%; 1.54%, 0.43%. The analytical recovery of three different con- centration was 99.2%, 102.9%; 100.9%, 101.8%; 97.5%,100.5%, with RSD was 0.84%, 0.31%; 0.20%,1.70%; 0.18%,0.12%. It was no less than 4.22 mg mg in per granule of the total content of Costunolide and Dehydroeostus lactone. Conclusion Regard Costunolide and Dehydrocostus lactone as a target of determining the content, using highly-effective liquid chromatography to measure it, the accuracy is high, the specificity is better, the reproducibility is good.