复方穿心莲片中2种成分含量测定及质量评价

Simultaneous Determination of Andrographolide,Dehydroandrographolide in Fufang Chuanxinlian Tablets and Quality Evaluation

目的:基于对照制剂,结合多组分含量测定,建立复方穿心莲片质量评价新模式。方法:采用Waters XBridge C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈-水(27∶73)为流动相,流速1.0 mL·min^(-1),柱温35℃,检测波长225 nm和254 nm,同时测定复方穿心莲片中穿心莲内酯和脱水穿心莲内酯的含量。按处方及标准工艺制备复方穿心莲片对照制剂,并以上述2个成分的含量测定结果作为随行对照,开展样品的质量评价。结果:穿心莲内酯和脱水穿心莲内酯分别在0.002189~0.2189 mg·mL^(-1)和0.002044~0.2044 mg·mL^(-1)浓度范围内与峰面积呈良好的线性关系,相关系数r均为1.0000;平均回收率(n=6)分别为96.3%(RSD=1.1%)和95.3%(RSD=0.3%)。根据对照制剂及样品的测定结果,拟定适当的限度标准并将满足限度要求的复方穿心莲片的质量分为三级,10个厂家40批样品中,一、二级品各为4批,均占样品总量的10%;未满足限度要求的不合格品为25批,占样品总量的62.5%,可见复方穿心莲片的产品质量亟待提高且不同厂家产品的质量差异较大。结论:所建立的质量评价模式可初步反映复方穿心莲片的质量优劣,可为该品种的质量监管提供科学可靠的技术参考。

Objective:On account of the reference drug,a new quality evaluation model for Fufang Chuanxinlian tablets(FCT)was established based on multi-component determination.Methods:Simultaneous determination of andrographolide and dehydroandrographolide in FCT was performed on a Waters XBridge C_(18) column(4.6 mm×250 mm,5μm)with acetonitrile-water(27∶73)as the mobile phase at a flow rate of 1.0 mL·min^(-1).The column temperature was 35℃and the detection wavelength was 225 nm and 254 nm.To evaluate the quality of the samples,the reference drug of FCT was prepared according to prescription and standard technology,which was used as a companion control to determine the above two components in the samples.Results:Andrographolide and dehydroandrographolide showed good linear relationships between the concentration and the peaks area in range of 0.002189-0.2189 mg·mL^(-1) and 0.002044-0.2044 mg·mL^(-1),respectively(r=1.0000 both).The average recovery(n=6)was 96.3%(RSD=1.1%)and 95.3%(RSD=0.3%),respectively.According to the test results of reference drug and samples,an appropriate quality limit of FCT was developed and the qualified samples were divided into three grades.Among 40 batches of samples from 10 manufacturers,there were 4 batches of grade Ⅰ and grade Ⅱ products respectively,which both accounted for 10%of the total samples,and 25 batches of unqualified samples accounted for 62.5%.The research showed that the quality of FCT should be improved immediately and there were significant differences among the products from different manufacturers.Conclusion:The research results show that the established quality evaluation model can preliminarily reflect the quality situation of FCT and provide a scientific and reliable technical support for the quality supervision.