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10 protocols using drx 300 mhz

1

NMR Analysis of HPLC-Isolated Limonene

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The nuclear magnetic resonance (NMR) spectra of the HPLC isolated fraction of limonene were recorded on a DRX-300 MHz Bruker, Switzerland (300 MHz for 1H, 75 MHz for 13C), NMR spectrometer in CDCl3. Chemical shifts were expressed in ppm downfield from TMS taking as an internal standard. Data are given in the following order: d value, multiplicity (s, singlet; d, doublet; t, triplet; q, quartet; m, multiplet; br, broad), number of protons, coupling constants J is given in Hz.
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2

Spectroscopic Analysis of Synthesized Compounds

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All analytical grade chemicals were purchased from Sigma-Aldrich. Nicolet iS5 (Thermo Scientific FTIR) was used to record the FTIR spectra (4000-400 cm−1) of the synthesised compounds. The 1H and 13C NMR spectra were analysed using a Bruker DRX-300 MHz and 75 MHz instrument. The percentages of N, S, H, and C were ascertained using a Vario EL III element analyser. PerkinElmer GCMS (Clarus sq8) was used to record the mass spectra.
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3

Synthesis and Characterization of Organic Compounds

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All chemical were purchased from the Merck, Sigma-Aldrich, and used without further purification. Solvent were dried and distilled prior to use. Merck pre-coated silica gel plates with a fluorescent indicator were used for analytical TLC. Flash column chromatography was performed using silica gel (Merck). Ethyl acetate – hexane was used as a eluting solvent for TLC and column chromatography. Melting points were recorded in open capillary tubes and were uncorrected. The FT-IR spectra (KBr) were recorded on a Shimadzu 8201pc (4000–400 cm−1) spectrometer. The 1H NMR (Proton Nuclear Magnetic Resonance Spectra) were obtained on a Bruker DRX-300 MHz and those of 13C NMR (Carbon Nuclear Magnetic Resonance Spectra) were recorded on a Bruker DRX-75 MHz advance spectrometer. Chemical shifts of 1H and 13C Nuclear Magnetic Resonance spectra were expressed in ppm in downfield from tetramethylsilane. Mass spectrum (EI) was recorded on a Jeol JMS D-300 spectrometer operating at 70 eV. The elemental analysis (C, H, N, and S) were recorded using an Elemental analyzer model (Varian EL III) and agreed with the calculated values.
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4

NMR, FT-IR, and Elemental Analysis

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1H and 13C NMR analyses were carried out using Bruker DRX-300 MHz and 75 MHz spectrometers. FT-IR (KBr) spectra, ranging from 4000–400 cm−1, were obtained on a Nicolet iS5 instrument from Thermo Scientific. The silica gel plates were purified using thin-layer chromatography. A Varioel III elemental analyser was used to calculate the percentages (%) of C, H, S, and N. Mass spectra were recorded on a Clarus 690 – SQ8MS (EI) instrument from PerkinElmer GCMS.
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5

Synthesis and Characterization of Novel Compounds

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All reagents were commercial compounds with high purity. Argon atmosphere was employed for all reactions. Triethylamine (Et3N) and dichloromethane (DCM) were dried by distillation over NaOH and CaH2, respectively. Acetonitrile (MeCN) was purchased anhydrous. Analytical thin layer chromatography (TLC) was carried out on aluminum plates with Merck Silicagel 60 F254 and visualized by UV irradiation (254 nm). Flash column chromatography was performed with Merck Kieselgel 60 (230–400 mesh). Proton nuclear magnetic resonance (1H NMR) spectra were recorded in DMSO at room temperature in a Bruker DRX-300 MHz device. The proton spectra was reported as follows: chemical shifts (δ) in ppm (number of protons, multiplicity, coupling constant J in Hz, assignment). Carbon nuclear magnetic resonance (13C NMR) were recorded in DMSO-d6 at room temperature using the same spectrometers at 75 MHz. The infrared spectra (IR) were obtained using an Agilent Technologies Cary 630 FTIR spectrophotometer from a thin film. Purity of the compounds was studied by high-performance liquid chromatography (HPLC), coupled with high-resolution mass spectrometry (HRMS) electrospray with positive mode detection for mass determination, using a mass spectrometer with a quadrupole time-of-fight analyzer (QTOF) model QSTAR pulsar I (Applied Biosystems, Waltham, MA, USA).
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6

Synthesis and Characterization of Coumarins

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The chemicals 7-hydroxy-4-methylcoumarin, tyrosinase, and bergapten were purchased from Sigma-Aldrich and used without further purification. Melting points were recorded in open capillary tubes and were uncorrected. The IR spectra (KBr) were recorded in KBr on a Shimadzu 8201 pc (4000–400 cm−1). The 1H NMR and 13C NMR spectra were recorded on a Bruker DRX-300 MHz. Elemental analysis (C, H, and N) was performed using an Elemental analyzer model (Varian EL III). The purity of the compounds was checked via thin layer chromatography (TLC) with silica gel plates.
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7

Synthesis of Novel Chitosan Derivatives

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All the substance and reagents such as chitosan (degree of deacetylation - 75%, Mw141 KDa), acetic acid, AEEA, chlorosulfonicacid, aromatic aldehydes, ethanol and DMF are purchased from Merck. The melting points of synthesized substances were evaluated in open capillary tubes, and were uncorrected. The FT-IR spectra were recorded in KBr on a Shimadzu 8201pc (4,000–1,000 cm−1). The 1H-NMR and 13CNMR spectra were recorded on a Bruker DRX-300 MHz. To obtain NMR spectra, the product was dissolved in DMSO-d6. TLC was used to assess the purity of the compounds, with silica-gel and 60F254 aluminium sheets as the adsorbent.
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8

Spectroscopic Analysis of Organic Compounds

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All chemicals were purchased from Merck and Sigma–Aldrich, and were used without further purification. Pre-coated silica gel plates impregnated with a fluorescent indicator were used for analytical TLC. An ethyl acetate/hexane solvent mixture was used as the eluent for both TLC and column chromatography. The FT–IR spectra were recorded using KBr pellets on a Shimadzu 8201pc spectrometer operating between 4000 and 400 cm−1. The 1H and 13C NMR spectra were obtained on Bruker DRX-300 MHz and Bruker DRX-75 MHz Avance spectrometers, respectively, and the resulting chemical shifts were expressed in ppm using tetramethylsilane as the internal standard. JEOL JMS D-300 spectrometer was used to analysis the mass spectra (EI) all compounds. Elemental analysis (C, H, N, and S) was conducted using a Varian EL III elemental analyzer.
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9

Comprehensive Chemical Analysis Protocol

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Spectrophotometer lambda 850 was used to check all bioactivities. FT-IR (4000–400 cm–1) was recorded by Shimadzu 8201PC analysis. Bruker DRX-300 MHz, 75 MHz was used for the analysis of 1H and13C NMR spectra. A Vario EL III  organic element analyzer was used to analyze the percentage (%) elements (C, H, N and S) presents in synthesised compounds.
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10

Phytochemical Analysis by Spectroscopic Methods

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Infra red (IR) spectrum was obtained by Perkin-Elmer RX-1 spectrophotometer using Br pellets or in neat. ESI-MS and HR-ESIMS were recorded on Jeol SX 102/DA-6000 spectrometer at 70 eV with direct inlet system. 1D and 2D NMR spectra were recorded on AVANCE, Bruker DRX 300 MHz spectrometers using TMS as internal standard for recording chemical shift. Silica gels of different mesh size (60-120 and 230-400 mesh) wereused for normal as well as flash chromatography. HPLC was run on Shimadzu, UV SPD-10 AVP system, using RP-18 (Shimpack RRC-ODS 20 mm x 25 cm) columns. TLC was run on precoated silica gel 60 F 254 and RP-18 F 254 (Merck) . Detection was done under UV light, by iodine vapours or by spraying with10% methanolic sulphuric acid followed by heating. All the solvents were purified prior to use. Plant material was grounded using a spice grinder. Pressurized hot water extraction was undertaken employing household coffee maker of Inalsa Company (Model Cafe Aroma)
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