Content Determination of 7 Related Substances in Solifenacin Succinate Raw Material by HPLC with Principal Component Self-control with Correction Factor
- VernacularTitle:HPLC-加校正因子的主成分自身对照法同时测定琥珀酸索利那新原料药中7种有关物质
- Author:
Qing GUO
1
,
2
;
Li LIU
2
;
Zigui ZHOU
2
;
Yong QIN
1
Author Information
1. College of TCM，China Pharmaceutical University，Nanjing 211198，China
2. Jiangsu Shenlong Pharmaceutical Co.，Ltd.，Nanjing 210046，China
- Publication Type:Journal Article
- Keywords:
Solifenacin succinate;
Raw material;
Related substance;
HPLC;
Correction factor
- From:
China Pharmacy
2019;30(11):1481-1486
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE： To establish method for simultaneous determination of 7 related substances in solifenacin succinate raw material. METHODS： HPLC method was adopted. The determination was performed on Thermo Hypersil ODS C18 column with mobile phase consisted of 0.02 mol/L KH2PO4 （0.02％ triethylamine， pH＝3.0）-acetonitrile （gradient elution） at the flow rate of 1.2 mL/min. The detection wavelength was set at 210 nm， and column temperature was 40 ℃. The sample size was 20 μL. The regression equation of solifenacin succinate and impurity A， C， D， I， J， K， L were drawn. Correction factors of impurities to solifenacin succinate were calculated with slope. The contents of impurities A， C， D， I， J， K and L were determined in 3 batches of solifenacin succinate raw material. RESULTS： The linear ranges of impurity A， C， D， I， J， K and L were 0.148 1-0.740 3， 0.142 9-0.714 5， 0.141 1-0.705 6， 0.148 9-0.744 6， 0.152 0-0.759 9， 0.137 9-0.689 6， 0.020 0-0.100 0 μg/mL （r＝0.999 8， 0.999 9 or 1.000 0）， respectively. The relative correction factors were 0.51， 0.40， 0.41， 0.91， 0.47， 0.85， 1.23. The limits of detection were 0.049 3， 0.047 6， 0.047 0， 0.048 1， 0.050 7， 0.046 0， 0.006 7 μg/mL. The quantification limits were 0.148 1， 0.142 9， 0.141 1， 0.148 9， 0.152 0， 0.137 9， 0.020 0 μg/mL， respectively. RSDs of precision， stability （24 h） and reproducibility tests were all lower than 5.0％ （n＝6）. Average recoveries were 101.09％， 97.58％， 93.77％， 98.56％， 99.68％， 97.07％ and 93.54％； RSDs were 0.75％ ， 0.51％， 0.47％， 0.84％， 0.70％， 0.75％， 1.21％ （n＝9）. The contents of impurity I in 3 batches of solifenacin succinate raw material were 0.015％-0.018％， other impurities were not detected. CONCLUSIONS： The method is sensitive， accurate and reliable， which can be used to determine the related substances of solifenacin succinate raw material.
