胃灵颗粒质量分析  

Quaily Analysis of Weiling Granules

作　　者：田金苗 孔令锋 陈婧 Tian Jinmiao;Kong Lingfeng;Chen Jing(Liaoning Provincial Institute for Drug Control,Shenyang 110036,China)

机构地区：[1]辽宁省药品检验检测院,沈阳110036

出　　处：《中国药师》2018年第10期1874-1878,共5页China Pharmacist

基　　金：2017年国家药品评价抽检项目(编号:2017026)

摘　　要：目的:对167批次胃灵颗粒样品进行标准检验及探索性研究,对该品种的质量及标准状况作出总体分析及评价。方法:TLC法鉴别处方中的白术; HPLC法建立指纹图谱及芍药苷、延胡索乙素、甘草酸铵的含量测定,采用Agilent Poroshell120,SB-C_(18)色谱柱(100 mm×4. 6 mm,2. 7μm),流动相乙腈-0. 1%磷酸梯度洗脱,流速:1. 8 ml·min^(-1),进样量:3μl;酸碱滴定法测定制酸力。结果:白术TLC鉴别阴性对照无干扰;指纹图谱的精密度、重复性与稳定性良好,相对保留时间和相对峰面积的RSD均<3. 0%,指纹信息完整;含量测定方法中芍药苷、甘草酸铵和延胡索乙素的线性范围分别为0. 057～0. 568μg (r=0. 999 9)、0. 035～0. 353μg (r=0. 999 9)和4. 244×10^(-3)～42. 440×10-3μg(r=0. 999 9),回收率分别为99. 3%,(RSD=1. 0%),100. 0%(RSD=0. 8%),99. 8%(RSD=1. 2%)(n=6);制酸力的回收率为99. 5%,RSD=0. 5%(n=6)。结论:探索性研究增加了标准的专属性、可控性及安全性,为进一步修订药品标准、控制药品质量提供参考。Objective： To analyze 167 batches of Weiling granules according to the quality standard and exploratory research,and evaluate the overall quality and standard condition of the preparation. Methods： A TLC method was established for the identification of Atractylodis macrocephalae Rhizoma; an HPLC method was established for the fingerprint and the content determination of paeoniflorin,tetrahydropalmatine and ammonium glycyrrhizinate. An Agilent Poroshell120,SB-C18 analytical column（ 100 mm × 4. 6 mm,2. 7 μm）was employed with gradient elution of acetonitrile-0. 1% phosphoric acid as the mobile phase at the flow rate of 1. 8 ml·min^-1,and the sample size was 3 μl. Acid base titration method was used for measuring acid-neutralizing capacity. Results： No interference from the negative controls was shown to the TLC identification of Atractylodis macrocephalae Rhizoma. The fingerprint exhibited better separation of each peak. The precision,reproducibility and stability of the method were good,and the RSDs of the relative retention time and relative peak area were less than 3. 0%. The linear range of paeoniflorin,tetrahydropalmatine and ammonium glycyrrhizinate was 0. 057-0. 568 μg（ r = 0. 999 9）,0. 035-0. 353 μg（ r = 0. 999 9） and 4. 244 × 10^-3-42. 44 × 10^-3μg（ r = 0. 999 9）,respectively,and the average recovery was 99. 3%（ RSD = 1. 0%,n = 6）,100. 0%（ RSD = 0. 8%,n = 6） and 99. 8%（ RSD = 1. 2%,n = 6）,respectively.The average recovery of acid-neutralizing capacity was 99. 5%（ RSD = 0. 5%,n = 6）. Conclusion： Exploratory research increases the specificity,controllability and safety of the standards,which provides reference for the further drug standards revision and the drug quality control.

关 键 词：胃灵颗粒 质量分析 指纹图谱 芍药苷 延胡索乙素 甘草酸铵 

分 类 号：TQ460.72[医药卫生—药物分析学]