反相高效液相色谱法测定川楝子中川楝素含量

Determination of Toosendanin in Melia Toosendan by RP- HPLC

目的：建立测定川楝子药材中川楝素含量的反相高效液相色谱（RP－HPLC）法，并与高效液相色谱－质谱（HPLC－MS）法进行比较。方法色谱柱为Agilent TC－C18柱（250 mm ×4.6 mm，5μm），流动相为乙腈－水（25：75），检测波长为210 nm，柱温为35℃，流速为1 mL／min，进样量为10μL。结果川楝素质量浓度在0.036~0.280 g／L范围内与峰面积线性关系良好（ r=0.9998），平均回收率为102.38%，RSD=3.89%（ n=6）。应用RP－HPLC和HPLC－MS法检测3批次药材川楝素含量分别为0.17%，0.17%，0.18%和0.18%，0.18%，0.19%。结论所建立方法使用仪器普及率高，操作简单，成本低，检测精密度和准确度满足应用要求。与HPLC－MS法比较，RP－HPLC法检测含量稍高，基层药品检验部门和一般制药企业可利用该方法对川楝素进行质量控制。

Objective To establisb a RP-HPLC metbod for tbe determination of tbe toosendanin content in Melia toosendan and to compare it witb tbe HPLC-MS. Methods Tbe cbromatograpbic conditions were as follows：tbe Agilent TC-C18 column（250 mm × 4. 6 mm,5 μm）,tbe mobile pbase of acetonitrile-water（25 ：75）at a flow rate of 1 mL/min,tbe detection wavelengtb of 210 nm and tbe sample size of 10 μL. Results Tbe linear range of toosendanin in Melia toosendan was 0. 036-0. 280 g/L（ r=0. 999 8）. Tbe av-erage recovery rate was 102. 38%,RSD=3. 89% （ n=6 ） . Tbe toosendanin contents in 3 batcbes of medicinal material determined by RP- HPLC and HPLC-MS were 0. 17%,0. 17%,0. 18% and 0. 18%,0. 18%,0. 19% respectively. Conclusion Tbe establisbed metbod bas bigb popularizing rate for using instrument,is easy to operate,bas low cost,its detection precision and accuracy meet tbe application requirements. Compared witb HPLC-MS,tbe detected content of RP-HPLC is sligbtly bigber. Tbe primary drug inspection department and general pbarmaceutical enterprise can use tbis metbod to conduct tbe quality control on toosendanin.