新安软胶囊质量标准研究

Quality standard for Xin'an Soft Capsules

目的研究新安软胶囊(椒目仁油、水飞蓟素等)的质量控制方法。方法采用TLC法对制剂中水飞蓟宾进行薄层鉴别;采用C18柱(5μm,4.6 mm×250 mm),流动相为甲醇-1%冰醋酸(50∶50),检测波长为288 nm的HPLC色谱条件来测定制剂中水飞蓟宾的含有量;采用以涂布浓度为15%的丁二酸二乙二醇聚酯(DEGS)不锈钢填充柱(2 m×3 mm),进样口温度为300℃,柱温为180℃,检测器为氢焰离子化检测器(温度320℃),载气为高纯氮(体积流量40 mL/min)的GC色谱条件来测定制剂中油酸、亚油酸与α-亚麻酸的含有量。结果水飞蓟宾的薄层鉴别具有较好的专属性;水飞蓟宾的回归方程:Y=11 264 551X-122 560,r=0.999 2,线性范围为0.016 4～0.822 0 mg/mL;平均回收率为99.06%,RSD值为0.57%;油酸的回归方程:Y1=0.640 5X1+0.155 1,r1=0.999 8,线性范围为3.68～23.02 mg/mL,校正因子及其RSD值分别为1.03%、1.73%;平均回收率为98.37%,RSD值为0.65%;亚油酸的回归方程:Y2=0.550 2X2+0.094 1,r2=0.999,线性范围为2.728～17.050 mg/mL,校正因子及其RSD值分别为1.21%、2.90%;平均回收率为98.89%,RSD值为0.31%;α-亚麻酸的回归方程:Y3=0.523 4X3+0.041 4,r3=0.999,线性范围为1.95～12.18 mg/mL,校正因子及其RSD值分别为1.28%、2.62%;平均回收率为99.20%,RSD值为0.60%。结论所建立的方法可用于该制剂的质量控制。

AIM To establish the quality standard for Xin＇an Soft Capsules （ seed oil of Zanthoxylum bungea- Mum Maxim, silybin, etc. ）. METHODS Silybin in the preparation was identified by TLC. And the content of silybin in the preparation was determined by HPLC on C18 column （5 um, 4.6 mm × 250 mm）, with mobile phase of methanol-1% acetic acid （50 ： 50） and detection wavelength of 288 nm. The contents of oleic acid, linoleic acid and a-linolenic acid in the preparation were determined by GC on a coating cloth concentration of 15% DEGS stainless steel packed column （2 m × 3 mm）, with inlet temperature of 300 ℃, column temperature of 180 22, flame ionization detector temperature of 320 22, and high purity nitrogen as carrier gas （ flow rate of 40 mL/min）. RESULTS Silybin TLC had good specificity. Silybin regression equation was Y = 11 264 551X - 122 560 and r = 0. 999 2 in the concentration range of 0. 016 4-0. 822 0 mg/mL, and average recovery was 99.06% , and its RSD was 0.57%. Oleic acid regression equation was Y1 = 0. 640 5X1 ＋ 0. 155 1 and r1 = 0. 999 8 in the concentration range of 3.68-23.02 mg/mL, and correction factor and its RSD value were 1.03 and 1.73% , respectively. And the average recovery was 98.37% , and its RSD value was 0. 65%. Linoleic regression equation was Y2 = 0. 550 2X2 ＋ 0. 094 1 and r2 = 0. 999 in the concentration range of 2. 728-17.050 mg/mL, and the correction factor and its RSD value were 1.21 and 2. 90% , respectively. And average recovery was 98.89% and its RSD value was 0. 31%. a-linolenic acid in the regression equation was Y3 =0. 523 4X3 ＋0. 041 4 and r3 =0. 999 in the concentration range of 1.95-12. 18 mg/mL, and the correction factor and its RSD value were 1.28 and 2.62% , respectively. And average recovery was 99.20% and its RSD was 0.60% . CONCLUSION The established method can be used for quality control of the preparation.