HPLC波长切换法同时测定沉香舒气丸中9种成分的含量

Simultaneous Determination of Nine Compositions in Chenxiang Shuqi Wan by HPLC Wavelength Switching Method

关键词:  沉香舒气丸  波长切换法  高效液相色谱法  化学成分

Key words:  Chenxiang Shuqi Wan  wavelength switching method  HPLC  chemical composition

摘要:

目的 建立并验证同时测定沉香舒气丸中α-香附酮、木香烃内酯、去氢木香内酯、原阿片碱、延胡索乙素、紫堇碱、四氢小檗碱、和厚朴酚、厚朴酚含量的HPLC波长切换方法。方法 采用Kromasil Eternity C₁₈色谱柱（250 mm×4.6 mm，5 μm）；流动相A为甲醇-乙腈（1：1），流动相B为0.1%磷酸溶液，梯度洗脱；检测波长分别为250，225，280，294 nm；体积流量0.9 mL·min^-1；柱温30℃。结果 9种成分α-香附酮、木香烃内酯、去氢木香内酯、原阿片碱、延胡索乙素、紫堇碱、四氢小檗碱、和厚朴酚、厚朴酚分别在5.79~115.80，7.86~157.20，9.68~193.60，1.07~21.40，3.09~61.80，3.77~75.40，2.09~41.80，15.77~315.40，19.86~397.20 μg·mL^-1内线性关系良好；平均加样回收率分别为97.95%，98.97%，99.46%，97.37%，98.48%，98.10%，96.90%，99.35%和100.10%，RSD分别为1.35%，1.17%，0.89%，1.57%，1.27%，0.96%，1.09%，0.74%和0.90%。结论 所建立的测定方法操作便捷、重复性好，可用于沉香舒气丸的质量控制。

Abstract:

OBJECTIVE To develop and validate an HPLC wavelength switching method for detemining contents of α-cyperone, costunolide, dehydrocostuslactone, protopine, tetrahydropalmatine, corydaline, tetrahydroberberine, honokiol and magnolol in Chenxiang Shuqi Wan. METHODS HPLC method was employed on a Kromasil Eternity C₁₈ chromatographic column(250 mm×4.6 mm, 5 µm). The mobile phase was methanol-acetonitrile(1：1)(A)-0.1% phosphoric acid solution(B) with gradient elution. The detection wavelengths were 250, 225, 280, 294 nm. The flow rate was 0.9 mL·min^-1, and the column temperature was 30 ℃. RESULTS The liner ranges of α-cyperone, costunolide, dehydrocostuslactone, protopine, tetrahydropalmatine, corydaline, tetrahydroberberine, honokiol and magnolol were within 5.79-115.80, 7.86-157.20, 9.68-193.60, 1.07-21.40, 3.09-61.80, 3.77-75.40, 2.09-41.80, 15.77-315.40, 19.86-397.20 μg·mL^-1. The average recovery rates were 97.95%, 98.97%, 99.46%, 97.37%, 98.48%, 98.10%, 96.90%, 99.35% and 100.10%, with RSD of 1.35%, 1.17%, 0.89%, 1.57%, 1.27%, 0.96%, 1.09%, 0.74% and 0.90%. CONCLUSION The method was easy to operate and repeatable, can be used for quality control of Chenxiang Shuqi Wan．