摘要
目的:建立高效液相色谱法同时测定参苓健体粉中欧前胡素、异欧前胡素、花椒毒酚、茯苓酸、去氢茯苓酸、去氢土莫酸、白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ9个成分的含量,并建立HPLC指纹图谱。方法:采用Agilent Zorbax SB-C_(18)(250 mm×4. 6 mm,5μm)色谱柱,以乙腈-水溶液作为流动相进行梯度洗脱,流速为0. 8 ml·min-1,柱温为30℃,切换波长300 nm、210nm、220 nm及275 nm。以去氢土莫酸为参照峰,用中药色谱指纹图谱相似度评价软件(2004A版)对12批参苓健体粉进行相似度分析。结果:欧前胡素、异欧前胡素、花椒毒酚、茯苓酸、去氢茯苓酸、去氢土莫酸、白术内酯Ⅰ、白术内酯Ⅱ、白术内酯Ⅲ的线性范围分别为4. 15～83. 00μg·ml^(-1)(r=0. 999 9)、5. 06～101. 20μg·ml^(-1)(r=0. 999 8)、6. 88～137. 60μg·ml^(-1)(r=0. 999 7)、8. 87～177. 40μg·ml^(-1)(r=0. 999 9)、4. 03～80. 60μg·ml^(-1)(r=0. 999 5)、7. 32～146. 40μg·ml^(-1)(r=0. 999 8)、3. 84～76. 80μg·ml^(-1)(r=0. 999 7)、3. 81～76. 20μg·ml^(-1)(r=0. 999 8)和5. 37～107. 40μg·ml^(-1)(r=0. 999 6),平均加样回收率分别为98. 9%,99. 3%,99. 8%,100. 8%,101. 1%,100. 3%,101. 3%,100. 5%和99. 9%。12批样品中9个有效成分的含量范围分别在0. 125 8～0. 127 9 mg·g^(-1)、0. 134 7～0. 136 7 mg·g^(-1)、0. 172 6～0. 174 1 mg·g^(-1)、0. 226 6～0. 228 1 mg·g^(-1)、0. 102 6～0. 104 5 mg·g^(-1)、0. 200 7～0. 202 2 mg·g^(-1)、0. 120 0～0. 121 2 mg·g^(-1)、0. 120 4～0. 122 0 mg·g^(-1)和0. 146 0～0. 147 9 mg·g^(-1)。12批参苓健体粉的相似度均在0. 98以上。结论:本研究建立了参苓健体粉的指纹图谱及多指标成分含量的测定方法,为该制剂的质量控制及深入研究奠定了基础。
Objective:To establish a determination method for the characteristic fingerprint of Shenling Jianti powder and to determine imperatorin,isoimperatorin,xanthotoxol,pachymic acid,dehydroporia acid,dehydrotonic acid,atractylodesⅠ,atractylodesⅡand atractylodesⅢin the preparation simultaneously.Methods:The analysis was carried out on an Agilent Zorbax SB-C18 analytical column(250 mm×4.6 mm,5μm)with gradient elution by acetonitrile-water,and the switching wavelengths were 314 nm,210 nm,220 nm and 275 nm.The column temperature was 30℃at the flow rate of 0.8 ml·min^-1.Similarity analysis of the 12 batches of preparations was used by Chinese medicine chromatographic fingerprint similarity evaluation software(2004 A version)with dehydrotonic acid as the reference peak.Results:The linear range of imperatorin,isoimperatorin,xanthotoxol,pachymic acid,dehydroporia acid,dehydrotonic acid,atractylodesⅠ,atractylodesⅡand atractylodesⅢwas 4.15-83.00μg·ml^-1(r=0.999 9),5.06-101.20μg·ml^-1(r=0.999 8),6.88-137.60μg·ml^-1(r=0.999 7),8.87-177.40μg·ml^-1(r=0.999 9),4.03-80.60μg·ml^-1(r=0.999 5),7.32-146.40μg·ml^-1(r=0.999 8),3.84-76.80μg·ml^-1(r=0.999 7),3.81-76.20μg·ml^-1(r=0.999 8)and5.37-107.40μg·ml^-1(r=0.999 6),and the average recovery was 98.9%,99.3%,99.8%,100.8%,101.1%,100.3%,101.3%,100.5%and 99.9%,respectively.The contents of 12 batches of preparations were 0.125 8-0.127 9 mg·g-1,0.134 7-0.136 7 mg·g-1,0.172 6-0.174 1 mg·g-1,0.226 6-0.228 1 mg·g-1,0.102 6-0.104 5 mg·g-1,0.200 7-0.202 2 mg·g-1,0.120 0-0.121 2 mg·g-1,0.120 4-0.122 0 mg·g-1 and 0.146 0-0.147 9 mg·g-1,respectively.The similarity of the 12 batches of preparations was greater than 0.98.Conclusion:The research has established a method for the characteristic fingerprint and multi-component determination of Shenling Jianti powder,which lays foundation for the quality control and further study of the preparation.
作者
吴雯
吴锐枫
康江丽
Wu Wen;Wu Ruifeng;Kang Jiangli(Department of Pharmacy,No.900 Hospital of PLA Joint Logistics Support Force,Fuzhou350000,China)
出处
《中国药师》
CAS
2019年第5期852-856,共5页
China Pharmacist
