Simultaneous determination of salidroside and tyrosol in Beagle dog plasma using UHPLC-MS/MS after pre-column dansyl chloride derivatization
10.16438/j.0513-4870.2016-0882
- VernacularTitle:柱前衍生化结合UHPLC-MS/MS法同时测定Beagle犬血浆中的红景天苷和酪醇
- Author:
Shuai CHEN
1
;
Yuan-yuan XIA
2
;
Guang-li WEI
2
;
Quan-sheng LI
2
;
Meng-jie LIU
1
;
Yong CHEN
1
;
Duan-yun SI
2
Author Information
1. Hubei Province Key Laboratory of Biotechnology of Chinese Traditional Medicine, Hubei Collaborative Innovation Center for Green Transformation of Bio-resources, Hubei University, Wuhan 430062, China
2. State Key Laboratory of Drug Delivery Technology and Pharmacokinetics, Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China
- Publication Type:ORIGINAL ARTICLES
- Keywords:
salidroside;
tyrosol;
dansyl chloride;
derivatization;
UHPLC-MS/MS;
pharmacokinetics
- From:
Acta Pharmaceutica Sinica
2017;52(2):296-301
- CountryChina
- Language:Chinese
-
Abstract:
A pre-column derivatization method combined with UHPLC-MS/MS was developed for the simultaneous determination of salidroside and tyrosol in Beagle dog plasma. After protein precipitation by acetonitrile, the liquid supernatant was treated with dansyl chloride under dark conditions at 60℃ for 30 min, and then, the sample solution was extracted using methyl tertiary butyl ether. The multiple reaction monitoring in positive ion mode was used for MS detection of the tested analytes with the specific ion transitions of m/z 534.2→372.0 for salidroside derivative, m/z 372.0→171.0 for tyrosol derivative and m/z 506.0→171.0 for arbutin derivative. The chromatograph separation was achieved on an ACQUITY UPLC® BEH C18 column (100 mm×2.1 mm, 1.7 μm) with a gradient mobile phase consisting of acetonitrile (0.1% formic acid)-water (10% acetonitrile, 0.1% formic acid) for 9 min. The assay showed a good linearity over the range of 0.02/0.1-20/10 μmol·L-1 with a lower limit of quantitation of 0.02 and 0.1 μmol·L-1 for salidroside and tyrosol in dog plasma, respectively. The intra-and inter-day precisions were all less than 8.68%, and the accuracy was within ±11.4%. The established method with a high sensitivity, good specificity and reliability was appropriate for simultaneous determination of salidroside and tyrosol in dog plasma and successfully applied to a pharmacokinetic study after intragastric administration of salidroside to Beagle dogs.
