jmb · title 5 september 2013⎪vol. 23⎪no. 9 fig. s5. h-nmr spectrum of acacetin (400 mhz, cd...

J. Microbiol. Biotechnol. (2013), 23(11), 1–5 http://dx.doi.org/10.4014/jmb.1610.10012 jmb UPLC- QTOF-MS analysis. Ultra-performance liquid chromatography (UPLC) analysis was performed using an ACQUITY UPLC system (Waters Corporation, Milford, MA, USA) equipped with a binary solvent delivery manager, photodiode array (PDA) and a sample manager coupled to a Micromass Q-TOF Premier mass spectrometer equipped with an electrospray interface (Waters Corporation). The methanol extract and the compounds isolated by column chromatography were analyzed by UPLC-QTOF-MS. The chromatographic separations were performed on a 2.1 × 100 mm, 1.7 μm ACQUITY HSS T3 C18 chromatography column. The column temperature was maintained at 35°C, and the mobile phases A and B comprised water with 0.1% formic acid and acetonitrile with 0.1% formic acid, respectively. The gradient duration program was: 0 min, 5% B; 0-1 min, 5% B; 1-8 min, 5-23% B; 8-12 min, 23-98% B; wash to 1.4 min with 98% B; and a 1.6 min recycle time. The flow rate was 0.4 ml/min. The mass spectrometer was operated in positive ion mode. N2 was used as the desolvation gas. The desolvation temperature was 350°C, the flow rate was 500 l/h, and the source temperature was 100°C. The capillary and cone voltages were 2700V and 27V, respectively. The data were collected for each test sample from 200 to 1,500 Da with 0.25-s scan time and 0.01-s interscan delay over 25-min analysis time. Leucine- enkephalin was used as the reference compound (m/z 556.2771 in the positive mode). Fig. S1. UPLC-QTof-MS chromatogram of isolated compounds from Agastache rugosa leaves.

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Page 1: jmb · Title 5 September 2013⎪Vol. 23⎪No. 9 Fig. S5. H-NMR spectrum of acacetin (400 MHz, CD OD). Fig. S6. C-NMR spectrum of acacetin (100 MHz, CD OD)

J. Microbiol. Biotechnol. (2013), 23(11), 1–5http://dx.doi.org/10.4014/jmb.1610.10012 jmb

UPLC- QTOF-MS analysis. Ultra-performance liquid

chromatography (UPLC) analysis was performed using an

ACQUITY UPLCTM system (Waters Corporation, Milford,

MA, USA) equipped with a binary solvent delivery

manager, photodiode array (PDA) and a sample manager

coupled to a Micromass Q-TOF PremierTM mass

spectrometer equipped with an electrospray interface

(Waters Corporation). The methanol extract and the

compounds isolated by column chromatography were

analyzed by UPLC-QTOF-MS. The chromatographic

separations were performed on a 2.1 × 100 mm, 1.7 µm

ACQUITY HSS T3 C18 chromatography column. The

column temperature was maintained at 35°C, and the

mobile phases A and B comprised water with 0.1% formic

acid and acetonitrile with 0.1% formic acid, respectively.

The gradient duration program was: 0 min, 5% B; 0-1 min,

5% B; 1-8 min, 5-23% B; 8-12 min, 23-98% B; wash to 1.4 min

with 98% B; and a 1.6 min recycle time. The flow rate was

0.4 ml/min. The mass spectrometer was operated in

positive ion mode. N2 was used as the desolvation gas. The

desolvation temperature was 350°C, the flow rate was

500 l/h, and the source temperature was 100°C. The

capillary and cone voltages were 2700V and 27V,

respectively. The data were collected for each test sample

from 200 to 1,500 Da with 0.25-s scan time and 0.01-s

interscan delay over 25-min analysis time. Leucine-

enkephalin was used as the reference compound (m/z

556.2771 in the positive mode).

Fig. S1. UPLC-QTof-MS chromatogram of isolated compounds from Agastache rugosa leaves.

Page 2: jmb · Title 5 September 2013⎪Vol. 23⎪No. 9 Fig. S5. H-NMR spectrum of acacetin (400 MHz, CD OD). Fig. S6. C-NMR spectrum of acacetin (100 MHz, CD OD)

2 Name et al.

J. Microbiol. Biotechnol.

Fig. S1. MS, MS/MS, UV and HREIMS data of tilianin.

Title 3

September 2013⎪Vol. 23⎪No. 9

Fig. S2. MS, MS/MS, UV and HREIMS data of acacetin.

4 Name et al.

J. Microbiol. Biotechnol.

Fig. S3. 1H-NMR spectrum of tilianin (400 MHz, DMSO-d6).

Fig. S4. 13C-NMR spectrum of tilianin (100 MHz, DMSO-d6).

Title 5

September 2013⎪Vol. 23⎪No. 9

Fig. S5. 1H-NMR spectrum of acacetin (400 MHz, CD3OD).

Fig. S6. 13C-NMR spectrum of acacetin (100 MHz, CD3OD).

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