IR spectrum was recorded on a Nicolet 6700 spectrometer (Thermo Scientific, Waltham, MA, USA). Optical rotation was measured on a PerkinElmer 241 MC polarimeter (PerkinElmer, Fremont, CA, USA). 1H and 13C NMR spectra were acquired on a Bruker DRX-500 spectrometer (Bruker Biospin AG, Fällanden, Germany). Chemical shifts (δ) are reported in ppm with reference to the solvent signals, and coupling constants (J) are in Hz. ESIMS spectra were recorded on a Finngan-MAT-95 mass spectrometer and HRESIMS spectra were recorded on an Agilent 1290–6545 UHPLC-QTOF mass spectrometer. Commercial silica gel (Qingdao Haiyang Chemical Co., Ltd., Qingdao, China, 200–300 and 300–400 mesh) and Sephadex LH-20 gel (Amersham Biosciences, Little Chalfont, UK) were used for column chromatography (CC). Precoated silica gel GF-254 plates (Sinopharm Chemical Reagent Co., Shanghai, China) were used for analytical TLC. Reversed-phase (RP) HPLC was performed on an Agilent 1260 series liquid chromatograph equipped with a DAD G1315D detector at 210 nm (Agilent, Santa Clara, CA, USA). An Agilent semipreparative XDB-C18 column (5 μm, 250 × 9.4 mm) was employed for the purification. All solvents used for CC and HPLC were of analytical grade (Shanghai Chemical Reagents Co., Ltd., Shanghai, China) and chromatographic grade (Dikma Technologies Inc., Lake Forest, CA, USA), respectively.
G1315d dad detector
Manufactured by Agilent Technologies
Sourced in United States, Germany
The G1315D DAD detector is a diode array detector designed for liquid chromatography (LC) applications. It provides high-performance detection and spectral analysis capabilities for a wide range of analytes. The core function of the G1315D is to detect and quantify compounds in liquid samples by measuring their absorbance at various wavelengths.
Automatically generated - may contain errors
Lab products found in correlation
Precoated silica gel gf 254 plates, by Sinopharm (2 mentions)
Semipreparative xdb c18 column, by Agilent Technologies (2 mentions)
Gpc p4000, by Phenomenex (2 mentions)
1260 hplc, by Agilent Technologies (2 mentions)
6120 quadrupolems detector, by Agilent Technologies (2 mentions)
241 mc polarimeter, by PerkinElmer (1 mentions)
1290 6545 uhplc qtof mass spectrometer, by Agilent Technologies (1 mentions)
Sephadex lh 20 gel, by Cytiva (1 mentions)
Nicolet 6700 spectrometer, by Thermo Fisher Scientific (1 mentions)
Drx 500 spectrometer, by Bruker (1 mentions)
1260 infinity 2, by Agilent Technologies (1 mentions)
Aviii nmr spectrometer, by Bruker (1 mentions)
Nicolet is50 spectrometer, by Thermo Fisher Scientific (1 mentions)
Agilent liquid chromatography series 1260, by Agilent Technologies (1 mentions)
Sephadex lh 20, by Cytiva (1 mentions)
Avance 3 600 mhz spectrometer, by Bruker (1 mentions)
Aviii 600 spectrometer, by Bruker (1 mentions)
Av 500, by Bruker (1 mentions)
Uv 2550 spectrometer, by Beckman Coulter (1 mentions)
Nicolet 380 ft ir instrument, by Thermo Fisher Scientific (1 mentions)
10 protocols using g1315d dad detector
1
Analytical Characterization of Compounds
2
Isolation and Characterization of Bioactive Compounds from AOE
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According to LC-MS analysis result, there were two dominant peaks in AOE appeared at tR = 72.3 min and tR = 83.3 min, respectively. Therefore, the isolation of these two compounds were carried out by various chromatographic techniques.
AOE (5.2 g) was applied to ODS gel (20–45 μM, Fuji Silysia Chemical Co., Ltd., Greenville, NC, USA) column eluting with MeOH/H2O (v/v, 1:9, 2:8, 3:7, 4:6, 5:5, 9:1, 1:0, each 400 mL) to obtain 10 fractions (Frs. 1–10). By analysis of the fractions, the two target compounds were contained in Fr. 3 and Fr. 6, respectively. Thereby, Fr. 3 was submitted to semi-preparative HPLC performed with an Agilent Technologies 1260 Infinity II equipped with an Agilent DAD G1315D detector (Agilent, CA, USA) (COSMOSIL π-NAP packed column, 10 × 250 mm, 5 μm, Cosmosil, Kyoto, Japan; 38% MeOH/H2O, v/v; flow rate 4.0 mL/min; UV detection at 210/280 nm) to get compound1 . Fr. 6 was repeatedly subjected to semi-preparative HPLC (π-NAP column; 42% MeOH/H2O, v/v; flow rate 4.0 mL/min; UV detection at 210/280 nm) to acquire compound 2 .
The isolated compounds were sent to Bruker AVIII NMR spectrometer (Bruker, Baden-Wurttemberg, Germany) to get 1H (500 MHz) and 13C NMR (125 MHz) spectra. Chemical shifts were referenced to the solvent residual peaks.
AOE (5.2 g) was applied to ODS gel (20–45 μM, Fuji Silysia Chemical Co., Ltd., Greenville, NC, USA) column eluting with MeOH/H2O (v/v, 1:9, 2:8, 3:7, 4:6, 5:5, 9:1, 1:0, each 400 mL) to obtain 10 fractions (Frs. 1–10). By analysis of the fractions, the two target compounds were contained in Fr. 3 and Fr. 6, respectively. Thereby, Fr. 3 was submitted to semi-preparative HPLC performed with an Agilent Technologies 1260 Infinity II equipped with an Agilent DAD G1315D detector (Agilent, CA, USA) (COSMOSIL π-NAP packed column, 10 × 250 mm, 5 μm, Cosmosil, Kyoto, Japan; 38% MeOH/H2O, v/v; flow rate 4.0 mL/min; UV detection at 210/280 nm) to get compound
The isolated compounds were sent to Bruker AVIII NMR spectrometer (Bruker, Baden-Wurttemberg, Germany) to get 1H (500 MHz) and 13C NMR (125 MHz) spectra. Chemical shifts were referenced to the solvent residual peaks.
3
Characterization of Chemical Compounds
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The IR spectrum was recorded on a Nicolet iS50 spectrometer (Thermo Fisher Scientific, Madison, WI, USA). Optical rotations were measured on a PerkinElmer 241MC polarimeter. 1H and 13C NMR spectra were acquired on a Bruker AVANCE III 600 MHz spectrometer. Chemical shifts are reported with the residual CHCl3 (δH 7.26 ppm; δC 77.16 ppm) as the internal standard for 1H and 13C NMR spectra. HRESIMS spectra were recorded on Agilent G6250 Q-TOF (Agilent, Santa Clara, CA, USA). Commercial silica gel (Qingdao Haiyang Chemical Co., Ltd., Qingdao, China, 200–300 mesh, 300–400 mesh) was used for column chromatography, and precoated silica gel GF254 plates (Sinopharm Chemical Reagent Co., Shanghai, China) were used for analytical TLC. Sephadex LH-20 (Amersham Biosciences, Piscataway, NJ, USA) was also used for column chromatography. Reverse-phase (RP) HPLC was performed on an Agilent 1260 series liquid chromatography equipped with a DAD G1315D detector at 210 nm (Agilent, Santa Clara, CA, USA). An Agilent semi-preparative XDB-C18 column (5 μm, 250 × 9.4 mm) was employed for the purification. All solvents used for column chromatography and HPLC were of analytical grade (Shanghai Chemical Reagents Co., Ltd., Shanghai, China) and chromatographic grade (Dikma Technologies Inc., Foothill Ranch, CA, USA), respectively.
4
Spectroscopic and Chromatographic Characterization
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1H, 13C and 2D NMR spectra were recorded on a Bruker AV-500 and Bruker AVIII-600 spectrometer (Bruker), and the chemical shifts were referenced to the solvent residual peaks. HRESIMS spectra were measured with an API QSTAR Pulsar mass spectrometer (Bruker). UV spectra were obtained on a Shimadzu UV-2550 spectrometer (Beckman, America). IR absorptions were obtained on a Nicolet 380 FT-IR instrument (Thermo) using KBr pellets. Optical rotation was measured on a Rudolph Autopol III polarimeter. HPLC analysis was performed with an Agilent Technologies 1260 Infinity equipped with an Agilent DAD G1315D detector, and the separation columns were YMC-pack C18 columns (5 mm, 250 mm × 4.6 mm). Semi-preparative HPLC was performed on reversed-phase columns (YMC-packed C18, 5 mm, 250 mm × 10 mm). Silica gel (60–80, 200–300 mesh, Qingdao Marine Chemical Co. Ltd.), ODS gel (20–45 mm, Fuji Silysia Chemical Co. Ltd.), MCI gel (75–150 mm, Mitsubishi Chemical Co. Ltd.) and Sephadex LH-20 (Merck) were used for column chromatography. TLC was conducted on precoated Silica gel G plates (Qingdao Marine Chemical Co. Ltd.), and the spots were detected by spraying them with 5% H2SO4 in EtOH followed by heating.
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1H, 13C and 2D NMR spectra were recorded on a Bruker AV-500 and Bruker AVIII-600 spectrometer (Bruker), and the chemical shifts were referenced to the solvent residual peaks. HRESIMS spectra were measured with an API QSTAR Pulsar mass spectrometer (Bruker). UV spectra were obtained on a Shimadzu UV-2550 spectrometer (Beckman, America). IR absorptions were obtained on a Nicolet 380 FT-IR instrument (Thermo) using KBr pellets. Optical rotation was measured on a Rudolph Autopol III polarimeter. HPLC analysis was performed with an Agilent Technologies 1260 Infinity equipped with an Agilent DAD G1315D detector, and the separation columns were YMC-pack C18 columns (5 mm, 250 mm × 4.6 mm). Semi-preparative HPLC was performed on reversed-phase columns (YMC-packed C18, 5 mm, 250 mm × 10 mm). Silica gel (60–80, 200–300 mesh, Qingdao Marine Chemical Co. Ltd.), ODS gel (20–45 mm, Fuji Silysia Chemical Co. Ltd.), MCI gel (75–150 mm, Mitsubishi Chemical Co. Ltd.) and Sephadex LH-20 (Merck) were used for column chromatography. TLC was conducted on precoated Silica gel G plates (Qingdao Marine Chemical Co. Ltd.), and the spots were detected by spraying them with 5% H2SO4 in EtOH followed by heating.
5
SEC Analysis of Kraft Lignin Molecular Weights
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SEC analysis (weight-average (Mw), number-average (Mn) molecular weights, and polydispersity (Mw/Mn)) of kraft lignins was carried out in an Agilent Technologies 1260 HPLC. The samples were analyzed at 254 nm (G1315D DAD detector, Agilent, Waldbronn, Germany) using two columns (Phenomenex) coupled in series (GPC P4000 and P5000, both 300 × 7.8 mm) and a safeguard column (35 × 7.8 mm). NaOH (0.05 M), pumped at a rate of 1 mL min−1, was employed as mobile phase at 25 °C for 30 min. Samples were dissolved at a final concentration of 0.5 g/L in NaOH (0.05 M). Polystyrene sulfonated standard (peak average molecular weights of 4210, 9740, 65,400, 470,000, PSS-Polymer Standards Service) were used for the calibration curve [31 (link)].
6
Quantitative Analysis of MGQD Extract Components
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The high concentration of MGQD extract (2 g crude herbs/mL) was determined using an Agilent 1,200 series HPLC system (Agilent Technologies, Palo Alto, CA, United States) equipped with a G1315D DAD detector and an Agilent 5 TC-C18 column (250 × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile (A) and 0.1% phosphoric acid solution (B) with a gradient elution as follows: 0–3 min for 15% A, 85% B; 3–45 min for 15–35% A, 85%–65% B. The detection wavelength was set at 275 nm, the flow rate was 1.0 ml/min, the loading volume was 10 μL and the column temperature was maintained at 30°C. According to the retention time and peak area of the reference standard, a total of 5 components of MGQD were detected, namely, puerarin, baicalin, wogonin, berberine chloride, and palmatine chloride. HPLC results are shown in Supplementary Figure S1 .
7
Synthesis and Purification of Compound 11h
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All solvents
were reagent grade or HPLC grade.
Unless otherwise noted, all materials were obtained from commercial
suppliers and used without further purification. All reactions were
performed under nitrogen. Melting points were obtained on a Mel-Temp
apparatus and are uncorrected. 1H NMR spectra were recorded
at 400 MHz. 13C NMR spectra were recorded at 100 MHz. The
HPLC solvent system consisted of distilled water and acetonitrile,
both containing 0.1% formic acid. Preparative HPLC purification was
performed on an Agilent 1200 series HPLC system equipped with an Agilent
G1315D DAD detector using a Phenomenex Luna 5 μm C18 (2) column
(21.2 mm × 250 mm, 5 μm). Analytical HPLC was performed
on an Agilent 1200 series HPLC system equipped with an Agilent G1315D
DAD detector (detection at 220 nm) and an Agilent 6120 quadrupole
MS detector. Unless otherwise specified, the analytical HPLC conditions
involve a gradient of 20% acetonitrile/80% water for 0.5 min followed
by an increase to 85% acetonitrile/15% water over 4 min and continuation
of 85% acetonitrile/15% water for 3.5 min with a Luna C18 column (2.1
mm × 50 mm, 3.5 μm) at a flow rate of 0.75 mL/min. All
final compounds tested were confirmed to be of ≥95% purity
by the HPLC methods described above. The model of compound11h bound to human DAAO (Figure 4 ) was generated using AutoDock Vina.30 (link)
were reagent grade or HPLC grade.
Unless otherwise noted, all materials were obtained from commercial
suppliers and used without further purification. All reactions were
performed under nitrogen. Melting points were obtained on a Mel-Temp
apparatus and are uncorrected. 1H NMR spectra were recorded
at 400 MHz. 13C NMR spectra were recorded at 100 MHz. The
HPLC solvent system consisted of distilled water and acetonitrile,
both containing 0.1% formic acid. Preparative HPLC purification was
performed on an Agilent 1200 series HPLC system equipped with an Agilent
G1315D DAD detector using a Phenomenex Luna 5 μm C18 (2) column
(21.2 mm × 250 mm, 5 μm). Analytical HPLC was performed
on an Agilent 1200 series HPLC system equipped with an Agilent G1315D
DAD detector (detection at 220 nm) and an Agilent 6120 quadrupole
MS detector. Unless otherwise specified, the analytical HPLC conditions
involve a gradient of 20% acetonitrile/80% water for 0.5 min followed
by an increase to 85% acetonitrile/15% water over 4 min and continuation
of 85% acetonitrile/15% water for 3.5 min with a Luna C18 column (2.1
mm × 50 mm, 3.5 μm) at a flow rate of 0.75 mL/min. All
final compounds tested were confirmed to be of ≥95% purity
by the HPLC methods described above. The model of compound
8
Molecular Weight Analysis of Lignin
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SEC analysis (weight-average (Mw), number-average (Mn) molecular weights, and polydispersity (Mw/Mn)) were carried out in an Agilent Technologies 1260 HPLC (equipped with a G1315D DAD detector (Agilent, Waldbronn, Germany)) at 254 nm. Previously, lignin samples were dissolved at a final concentration of 0.5 g L−1 in NaOH (0.05 M). Two columns (Phenomenex, Torrance, CA, USA) coupled in series (GPC P4000 and P5000, both 300 × 7.8 mm) and a safeguard column (35 × 7.8 mm) were used. The operational conditions were described elsewhere [52 (link)].
9
Purification and Characterization of Organic Compounds
10
Quantification of Antipyrine in Maternal and Fetal Samples
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Quantitation of the antipyrine Concentrations of antipyrine in maternal and fetal aliquots were measured using a modified highperformance liquid chromatography (HPLC) method previously described by Morck et al. 14 Briefly, protein was precipitated by the addition of 200 mL of ice-cold acetonitrile containing 10 mL/ mL of internal standard phenacetin to each 200 mL sample. Samples were centrifuged at 8000 rpm, and supernatants were run on an Agilent 1200 HPLC system equipped with a G1315D DAD detector (Agilent Technologies, Santa Clara, CA).
Antipyrine was analyzed using an HPLC method with a lower limit of quantification of 5 mg/mL. The HPLC analysis was performed at room temperature (22e25 C) using a reversephase, C18-based column (Waters Atlantis T3, Atlantis T3 Column, 100Å, ). The samples were run with a linear gradient ranging from 25% to 95% methanol water over 14 minutes at a flow rate of 0.3 mL/min; the injection volume was 10 mL and detection was performed using absorbance at 260 nm.
Antipyrine was analyzed using an HPLC method with a lower limit of quantification of 5 mg/mL. The HPLC analysis was performed at room temperature (22e25 C) using a reversephase, C18-based column (Waters Atlantis T3, Atlantis T3 Column, 100Å, ). The samples were run with a linear gradient ranging from 25% to 95% methanol water over 14 minutes at a flow rate of 0.3 mL/min; the injection volume was 10 mL and detection was performed using absorbance at 260 nm.
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