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15 protocols using ft ir tensor 27 infrared spectrophotometer

1

Comprehensive Analytical Characterization

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Optical rotations were measured on a Jasco P-1020 polarimeter. UV spectra were detected on a Shimadzu UV-2401PC spectrometer. IR spectra were determined on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr disks. 1D and 2D NMR spectra were recorded on DRX-500 spectrometers using TMS as an internal standard. Unless otherwise specified, chemical shifts (δ) were expressed in ppm with reference to the solvent signals. ESIMS and HR-EIMS analysis were carried out on Waters Xevo TQS and Waters AutoSpec Premier P776 mass spectrometers, respectively. Semi-preparative HPLC was performed on an Agile 1100 HPLC with a Zorbax SB-C18 (9.4 × 250 mm) column. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co., Ltd., PR China), and Amphichroic RP-18 gel (40–63 μm, Merck, Darmstadt, Germany) and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography.
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2

Analytical Techniques for Structural Elucidation

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Optical rotation and UV spectra were measured on a AUTOPOL VI automatic and a SHIMADZU UV-2700 UV–VIS instruments, respectively. CD data were recorded on an Applied Photophysics spectro-polarimeter. A Bruker FT-IR Tensor-27 infrared spectrophotometer was utilized for measuring the IR spectra (KBr disks). NMR spectra were collected on Bruker Ascend 500, 600, and 800 MHz instruments with various solvent (including CDCl3, methanol-d4, acetone-d6, and pyridine-d5) signals as referenced internal standards. An Agilent 1290 UPLC/6540 Q-TOF system was used for HRESIMS data. Crystallographic data of 1 and a mixture of 10 and 11 were obtained using a Bruker D8 QUEST diffractometer (λ = 1.54178 Å) with Cu Kα radiation. Silica gel, Sephadex LH-20, and MCI were applied as the packing materials for CC (column chromatography). Chiral analysis was performed on an Agilent 1100 instrument with a CHIRALPAK IC column (4.6 × 250 mm, 5 μm). A Hanbon Newstyle preparative HPLC instrument equipped with a SunFire Prep C18 column (10 × 250 mm, 5 μm) was used to purify compounds.
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3

Spectroscopic Characterization of Compounds

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Optical rotations were measured on a JASCO P-1020 polarimeter. UV spectra were detected on a SHMADZU UV-2401PC spectrometer. IR spectra were determined on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr disks. 1D and 2D NMR spectra were recorded on Bruker DRX-400, DRX-500, and DRX-600 spectrometers using TMS as an internal standard. Chemical shifts (δ) were expressed in ppm with reference to the solvent signals. ESI–MS and EI–MS (HR–EI–MS) analysis were carried out on Waters Xevo TQS and Waters AutoSpec Premier P776 mass spectrometers, respectively. Semi-preparative HPLC was performed on a Waters 600 with a COSMOSIL C18 (10 × 250 mm) column. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co., Ltd., People’s Republic of China), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by thin-layer chromatography (TLC) (GF254, Qingdao Marine Chemical Co., Ltd.), and spots were visualized by 10% sulfuric acid ethanol solution and dragendorff reagent.
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4

Spectroscopic Characterization of Chemical Compounds

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Optical rotations were obtained with a Jasco P-1020 Automatic Digital Polariscope. UV spectrum was measured with a Shi madzu UV2401PC spectrometer. IR spectra were obtained on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr pellets. 1H, 13C, and 2D NMR spectra were recorded on a Bruker AM-400, Bruker DRX-500 NMR and Bruker DRX-600 spectrometer with TMS as internal standard. ESI-MS and HR-EI-MS analysis were carried out on Waters Xevo TQS and Waters AutoSpec Premier P776 mass spectrometers, respectively. Semi-preparative HPLC was performed on an Agilent 1100 HPLC with a ZORBAX SB-C18 (9.4 × 250 mm) column. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co. Ltd., P.R. China), Sephadex LH-20 (GE Healthcare Bio-Xciences AB), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by TLC (GF 254, Qingdao Marine Chemical Co. Ltd., P.R. China), and spots were visualized by 10 % H2SO4-ethanol reagent.
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5

Spectroscopic Characterization of Natural Compounds

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Optical rotations were measured on a Jasco P-1020 polarimeter. UV spectra were recorded on a Shimadzu UV2401 PC spectrophotometer. IR spectra were determined on Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr discs. ECD spectra were recorded on an Applied Photophysics spectropolarimeter. 1D and 2D NMR spectra were recorded on Bruker AV 600 or 800 MHz spectrometers using TMS as an internal standard. Chemical shifts (δ) were expressed in ppm with reference to the solvent signals, and coupling constant (J) values were reported in Hz. HRESIMS data were measured using an Agilent 1290 UPLC/6540 Q-TOF mass spectrometer. Sephadex LH-20 (GE Healthcare, Uppsala, Sweden), Si gel (200–300 mesh, Qingdao Marine Chemical Co., Qingdao, People’s Republic of China), and RP-18 (50 μm, Merck, Germany) were used for column chromatography (CC). Semi-preparative HPLC was performed on an Agilent 1260 instrument with a ZORBAX SB-C18 column (9.4 × 250 mm, 5 μm). Fractions were monitored by Si gel GF254 (Qingdao Marine Chemical Co., China) or RP-18 F254 (Merck, Darmstadt, Germany) plates. Spots were visualized under UV light and by spraying with 10% H2SO4 in EtOH followed by heating.
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6

Isolation and Characterization of Natural Products

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Optical rotations were obtained with a Jasco P-1020 Automatic Digital Polariscope. UV spectra were measured with a Shi madzu UV2401PC spectrometer. IR spectra were obtained on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr pellets. 1H, 13C, and 2D NMR spectra were recorded on a Bruker DRX-400 NMR, Bruker DRX-500 NMR and Bruker DRX-600 spectrometer with TMS as internal standard. ESI-MS and HR-EI-MS analysis were carried out on Waters Xevo TQS and Waters AutoSpec Premier P776 mass spectrometers, respectively. Semi-preparative HPLC was performed on a Waters 600 HPLC with a COSMOSIL 5C18 MS-II (10ID × 250 mm) column. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co. Ltd., P.R. China), Sephadex LH-20 (GE Healthcare Bio-Xciences AB), RP-18 gel (20–45 μm, Fuji Silysia Chemical Ltd., Japan), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by TLC (GF 254, Qingdao Marine Chemical Co., Ltd., Qingdao), and spots were visualized by Dragendorff’s reagent.
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7

Detailed Analytical Techniques for Chemical Analysis

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IR spectra were measured on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr disks. Optical rotations were recorded on a JASCO P-1020 polarimeter. UV spectra were obtained with a Shimadzu UV-2401PC spectrometer. 1D and 2D NMR spectra were performed on a Bruker DRX-600 spectrometer using TMS as an internal standard. The chemical shifts (δ) were expressed in ppm with reference to the solvent signals. HREIMS and HRESIMS analysis were obtained from Waters Xevo TQS and Agilent G6230 TOF mass spectrometers, respectively. Single-crystal X-ray diffraction data were exhibited on a Bruker D8 QUEST diffractometer. Semi-preparative HPLC was performed on a Waters 1525 HPLC with a ZORBAX SB-C18 (9.4 × 250 mm) column. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co., Ltd., People’s Republic of China), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by TLC (GF 254, Qingdao Marine Chemical Co., Ltd.), and spots were visualized by heating Silica gel plates immersed in 10% H2SO4 in ethanol. Methanol (HPLC grade) and acetonitrile (HPLC grade) was purchased from CINC High Purity Solvents Co., Ltd (Shanghai, China). 4-Nitrophenyl-α-d-glucopyranoside (PNPG), α-glucosidase, PTP1B assay kit, quercetin, and acarbose were purchased from Sigma Chemical (Merck KGaA, Darmstadt, Germany).
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8

Isolation and Characterization of Natural Compounds

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Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co., Ltd., Qingdao, China), MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by TLC (GF 254, Qingdao Marine Chemical Co., Ltd. Qingdao, China), and spots were visualized by heating Silica gel plates immersed in 8% H2SO4 in ethanol. Semi-preparative HPLC was performed on Waters 2695 HPLC with a COSMOSIL C18 -MS-II (4.6ID × 250 mm) packed column. 1D and 2D NMR spectra were recorded on a Bruker DRX-600 spectrometer using TMS as an internal standard. Unless otherwise specified, chemical shifts (δ) are expressed in ppm with reference to the solvent signals. ESIMS and HRESIMS data were acquired on Agilent G6200 TOF mass spectrometer. Optical rotations were measured on a Jasco P-1020 polarimeter. UV spectra were recorded on a Shimadzu UV-2401PC spectrometer. IR spectra were recorded on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr disks.
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9

Spectroscopic Characterization of Compounds

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Optical rotations were measured on a JASCO P-1020 polarimeter. UV spectra were recorded on a Shimadzu UV-2401PC spectrometer. IR spectra were recorded on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr disks. 1D and 2D NMR spectra were recorded on a Bruker DRX-600 spectrometer using TMS as an internal standard. The chemical shifts (δ) were expressed in ppm with reference to the solvent signals. ESIMS and HR-ESIMS analysis were carried out on Waters Xevo TQS and Agilent G6230 TOF mass spectrometers, respectively. Preparative and semi-preparative HPLC were performed on Waters 1525 HPLC (column: SunFire OBD-C18, 19 × 250 mm) and Agilent 1100 HPLC (column: Zorbax SB-C18, 9.4 × 250 mm), respectively. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co., Ltd., People’s Republic of China), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by TLC (GF 254, Qingdao Marine Chemical Co., Ltd.), and spots were visualized by heating silica gel plates immersed in H2SO4 in ethanol.
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10

Analytical Methods for Natural Product Characterization

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1D and 2D NMR spectra were recorded on Bruker DRX-500 spectrometers using TMS as an internal standard. Chemical shifts (δ) were expressed in ppm with reference to the solvent signals. Optical rotations were measured on a JASCO P-1020 polarimeter. IR spectra were determined on a Bruker FT-IR Tensor-27 infrared spectrophotometer with KBr disks. UV spectra were detected on a SHMADZU UV-2401PC spectrometer. MS and HRMS analysis were carried out on Waters Xevo TQS and Waters AutoSpec Premier P776 mass spectrometers, respectively. Semipreparative HPLC was performed on a Waters 600 with a COSMOSIL C18 (10 × 250 mm) column. Silica gel (100–200 and 200–300 mesh, Qingdao Marine Chemical Co., Ltd., People’s Republic of China), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan) were used for column chromatography. Fractions were monitored by thin-layer chromatography (TLC) (GF254, Qingdao Marine Chemical Co., Ltd.), and spots were visualized by 10% sulfuric acid ethanol solution.
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