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Molecules 2017, 22(5), 667; doi:10.3390/molecules22050667

High-Throughput Determination of Sodium Danshensu in Beagle Dogs by the LCMS/MS Method, Employing Liquid-Liquid Extraction Based on 96-Well Format Plates

1
Shanghai Key Laboratory for Pharmaceutical Metabolite Research, School of Pharmacy, Second Military Medical University, Shanghai 200433, China
2
Department of Pharmaceutical Analysis, School of Pharmacy, China Pharmaceutical University, No. 24 Tong Jia Xiang, Nanjing 210009, China
3
Laboratory of Drug Metabolism & Pharmacokinetics, School of Medicine, Tongji University, No. 1239 Siping Road, Shanghai 200092, China
4
Department of Pharmacy, Branch of Shanghai First People’s Hospital, Shanghai 200081, China
5
Department of Clinical Pharmacy, Shanghai General Hospital, School of Medicine, Shanghai Jiao Tong University, No. 100 Haining Road, Shanghai 200080, China
*
Authors to whom correspondence should be addressed.
Academic Editor: Diego Muñoz-Torrero
Received: 22 March 2017 / Revised: 14 April 2017 / Accepted: 18 April 2017 / Published: 25 April 2017
View Full-Text   |   Download PDF [920 KB, uploaded 25 April 2017]   |  

Abstract

Sodium Danshensu (sodium d-(+)-β-(3,4-dihydroxyphenyl) lactate), one of the water-soluble ingredients in Salvia miltiorrhiza, exhibits potent relaxation of the coronary artery and anticoagulation effection. A high-throughput, rapid, and sensitive method combining liquid chromatography with electrospray ionization tandem mass spectrometry to determine the sodium danshensu in beagle dog plasma was developed and validated, using gallic acid as an internal standard (IS). Acidified plasma samples were extracted using 96-well liquid-liquid extraction, and were eluted on a CNW Athena C18 column (3 μm, 2.1 × 100 mm) by using a gradient mobile phase system of methanol and water (containing 0.2% formic acid). The mass spectrometric detection was achieved using negative ion electrospray ionization mode and monitoring the precursor→production combinations of m/z 197→135 for sodium danshensu and 169→125 for IS, in multiple reaction monitoring modes. Good linearity was achieved, and the linear range was 10–1000 ng/mL (R2 > 0.996) with a quantification limit of 10 ng/mL for sodium danshensu in beagle dog plasma. The intra- and inter-day precision (RSD) ranged from 2.1% to 9.0%. The accuracy (RE) was between −8.6% and 5.7% at all quality control levels. The validated method was successfully applied to the pharmacokinetics study of sodium danshensu in beagle dog plasma after intravenous injection and oral administration of sodium danshensu. View Full-Text
Keywords: Sodium Danshensu; pharmacokinetics; LC-MS/MS; 96-well liquid-liquid extraction; Beagle dogs Sodium Danshensu; pharmacokinetics; LC-MS/MS; 96-well liquid-liquid extraction; Beagle dogs
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MDPI and ACS Style

Jiang, J.; Zhao, X.; Li, X.; Wu, S.; Yu, S.; Lou, Y.; Fan, G. High-Throughput Determination of Sodium Danshensu in Beagle Dogs by the LCMS/MS Method, Employing Liquid-Liquid Extraction Based on 96-Well Format Plates. Molecules 2017, 22, 667.

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