UPE-HILIC-DAD-ESI-TOF/MS法测定山东产区丹参中丹酚酸类成分

doi:10.3976/j.issn.1002-4026.2019.05.004

Shandong Science ›› 2019, Vol. 32 ›› Issue (5): 38-45.doi: 10.3976/j.issn.1002-4026.2019.05.004

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Determination of salvianolic acids in Salvia miltiorrhiza Bge. from Shandong region by UPE-HILIC-DAD-ESI-TOF/MS

DONG Sha-sha^1,2, CHENG Su-pan¹, MA Tian-yu¹, LIU Wei¹, ZHANG Yu-jie³, WANG Xiao¹, LIU Dai-cheng⁴, ZHAO Heng-qiang^1*

1.Shandong Provincial Key Laboratory of TCM Quality Control Technology, Shandong Analysis and Test Center, Qilu University of Technology (Shandong Academy of Sciences), Jinan 250014, China; 2. Jinan Fruit Research Institute, China Federation of Supply and Marketing Cooperatives，Jinan 250014, China; 3. College of Life Science, Linyi University, Linyi 276005, China 4. College of Life Science, Shandong Normal University, Jinan 250014, China

Received:2019-07-23 Online:2019-10-20 Published:2019-10-08

Abstract

Abstract: A method involving ultrahigh pressure extraction-hydrophilic interaction chromatography-diode array detector-electrospray time-of-flight mass spectrometry (UPE-HILIC-DAD-ESI-TOF/MS) was developed in this study for determining the content of salvianolic acids in Salvia miltiorrhiza Bge.(Danshen) from Shandong region. The UPE conditions were optimized in detail through a single-factor experiment; analysis was performed based on a Waters XBridge Amide column with water solution (0.8% formic acid, 20 mmol/L ammonium formate, 30% acetonitrile, and 10% n-butanol)-acetonitrile (0.8% formic acid) as mobile phase, gradient elution, flow rate 0.8 mL/min, column temperature at 25°C, and detection wavelength 280 nm; various compounds were identified by DAD-ESI-TOF/MS and quantified by HILIC-DAD. Under optimized extraction conditions, the extraction rate of UPE method was significantly higher than that of ultrasonic assisted extraction and reflux extraction method; desirable separation effect could be achieved by HILIC method for the salvianolic acids in Salvia miltiorrhiza Bge. In combination with standard reference materials, compounds could be accurately identified using precise molecular weight information obtained by ESI-TOF/MS and ultraviolet absorption information acquired by DAD. Seven types of salvianolic acids (including salvianolic acid A, rosmarinic acid, protocatechuic aldehyde acid, ursolic acid, purple oxalic acid, and salvianolic acid B) were determined. The results showed that there was a good linear relationship between peak area and mass concentration of each compound(r=0.999 0~1.000 0), the concentration range of each compound were 0.311~0.438, 1.218~1.517, 0.104~0.147, 0.375~0.527, 0.303~0.401, 4.025~4.935, and 35.628~44.255 mg/g. This method features high extraction efficiency and good degree of separation, providing technical evidence for extraction, determination, and quality evaluation of salvianolic acids from Danshen.

Key words: Salvia Miltiorrhiza Bge., salvianolic acids, ultrahigh pressure extraction, hydrophilic interaction chromatography, ESI-TOF/MS

CLC Number:

R284.1

DONG Sha-sha, CHENG Su-pan, MA Tian-yu, LIU Wei, ZHANG Yu-jie, WANG Xiao, LIU Dai-cheng, ZHAO Heng-qiang. Determination of salvianolic acids in Salvia miltiorrhiza Bge. from Shandong region by UPE-HILIC-DAD-ESI-TOF/MS[J].Shandong Science, 2019, 32(5): 38-45.

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Determination of salvianolic acids in Salvia miltiorrhiza Bge. from Shandong region by UPE-HILIC-DAD-ESI-TOF/MS

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