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16 protocols using dichloromethane

1

Synthesis of Pyridyl-Substituted Styrene Derivatives

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Styrene (>99%) and all the para-substituted styrene derivatives (4-methylstyrene, 4-fluorostyrene), α-methylstyrene, Palladium (II) chloride (99%) and α,α’-dibromo-p-xylene were purchased from Sigma-Aldrich. 2,4,6-tri(4-pyridyl)−1,3,5-triazine was purchased from TCI Chemicals Pvt. Ltd. Solvents (dichloromethane, chloroform, dimethylformamide, methanol, acetone, n-hexane, ethyl acetate, diethyl ether) were purchased from SD Fine Chemicals. Analytical reagent (AR) grade solvents were used for chemical reactions and HPLC grade solvents were used for spectroscopic measurements. Other chemical reagents like hydrochloric acid, sodium bicarbonate etc. were purchased from Sigma-Aldrich. Heavy water (D2O; 99.9 atom %D) was procured from Sigma-Aldrich and used as supplied for the chemical reactions as well as for the NMR measurements.
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2

Cabozantinib Nanoparticle Formulation for HepG2 Cells

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Cabozantinib was a gift sample obtained from Neon Laboratories Ltd, Mumbai, India. Poly D, L-lactide, glycolide, polysarcosine, 2-ethyl hexanoate, methylene chloride, and diethyl ether was purchased from Sigma-Aldrich, Bengaluru, India. Dichloromethane, methanol, polyvinyl alcohol, and d-trehalose was purchased from Sd Fine-Chem Limited, Mumbai, India. Spectra Por S/P 2 Dialysis Membrane was a gift sample from Cole-Parmer®, Mumbai, India. From National Centre For Cell Science, Pune, India hepatocellular carcinoma cell line (HepG2) was obtained. Further, Dulbecco’s Modified Eagle Medium (DMEM), Hepatocyte Culture Medium (HHCM), Fetal bovine serum (FBS), tetrazolium salt and propidium iodide (PI), tetrazolium salt (3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT), 4’, 6 diamidino-2-phenylindole (DAPI), Dimethyl sulfoxide (DMSO), was purchased from HiMedia Laboratories Pvt Ltd, Mumbai, India.
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3

Polyphenylsulfone Membrane Fabrication

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Polyphenylsulfone (PPSu) was kindly supplied by Solvay Advanced Polymers, Milano, Italy, and served as the main polymer matrix for the fabrication of the membranes. Polyethylene glycol-600, magnesium sulfate, sodium sulfate, sodium hydroxide, potassium chloride, sodium azide, and glycerol were obtained from Merck, Rahway, NJ, USA and used as received. Chlorosulfonic acid, an important reagent in the synthesis of sulfonated polyphenylenesulfone (SPPSu), was also obtained from Merck, Rahway, NJ, USA. Titanium dioxide nanoparticles, which played a crucial role in enhancing the properties of the membranes, were obtained from Sigma–Aldrich, Rahway, NJ, USA. Sodium dodecyl sulfate (SDS), a surfactant, was also obtained from Sigma–Aldrich and used in the membrane preparation process. N-Methyl Pyrrolidone and dichloromethane were sourced from SD Fine-Chem Limited, Tamil Nadu, Chennai, India, and used as solvents in the synthesis and processing of the membranes. Millipore MQ purified water was used for the experiments and to prepare the gelation bath, ensuring the purity of the water used in the membrane fabrication process.
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4

Formulation and Evaluation of Ketorolac Tromethamine Tablets

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Ketorolac tromethamine was gift sample from Dr. Reddy's Laboratories, Ahmadabad, India. Ethyl cellulose (lot no. 02129) was obtained from Central Drug House (P) Ltd, New Delhi, India. Eudragit RS100 was obtained from Evonik Roehm (Germany). Microcrystalline cellulose, magnesium stearate, methanol, and dichloromethane were purchased from S.D. Fine Chemicals (Mumbai, India). All other chemicals were purchased from local sources.
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5

Nanoparticle Formulation and Characterization

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Low molecular weight heparin (Enoxaparin) was a gift sample from Gland Pharma Pvt. Ltd., (Hyderabad, India). Polylactide co-glycolide (PLGA) (50:50, 85:15) was purchased from PolySciTech, USA. Dichloromethane and polyvinyl alcohol (PVA) were purchased from SD Fine Chemicals Ltd. An ultraviolet (UV) - visible spectrophotometer from Thermo scientific was used. Qsonica probe sonicator, Cooling centrifuge Hittech MIKRO 220 R, Freeze dryer (Mini Lyodel) Chennai, India were used for formulation of Nanoparticles. A JSM-5200 scanning electron microscope (SEM), Japan, was used to study the surface morphology of nanoparticles. Zetasizer Nano ZS (Malvern Instruments, Malvern, United Kingdom) was used to measure the particle size and zeta potential of prepared nanoparticles. Differential scanning calorimeter from Shimadzu, Fourier transform infrared spectrophotometer (FTIR) from Perkin-Elmer and X-ray diffractometer, X-ray powder diffraction (XRPD) from PAN analytical were used. All other ingredients used in this study were of analytical grade.
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6

Terbinafine Hydrochloride Topical Formulation

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Terbinafine Hydrochloride (TH) was received from A.S Lifesciences, (Haryana, India). Other ingredients used were Polyvinyl Alcohol (PVA) (GS Chemical Testing & Chemical Industries, New Delhi, India); Ethyl Cellulose (EC) (Titan biotech Ltd., Rajasthan, India); Dichloromethane, Tween 80, Carbopol 940, and Ethanol (S.D. Fine Chemicals Ltd., Mumbai, India); TriEthanolamine (Loba Chemie, Mumbai; India). Analytical grade reagents were used for the research.
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7

Development of α-MNG Nanoformulation

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α-MNG (MW 410.46 g/mol; purity = 98%) was obtained from Sigma-Aldrich. PLGA [poly(D, L-lactide-co-glycolide)] lactide: glycolide (50:50) (Mw = 44,628 g/mol; viscosity, 0.71–1.0 dl/g) (Merck, India). Polyvinyl alcohol (PVA) was obtained from Sisco Laboratory (Mumbai, India) and Rhodamine B (RhB) from Sigma-Aldrich (St. Louis, MO, USA). The laboratory solvents, namely acetone, dichloromethane, acetonitrile, and deionized water, were procured from SD Fine Chemicals (Mumbai, India). LC-MS grade reagents, namely acetonitrile, methanol, ammonium acetate, ethyl acetate, glacial acetic acid, and water, were purchased from Sigma-Aldrich (St. Louis, MO, USA). The analytical grades of buffer reagents, i.e., phosphate-buffered saline (PBS), sodium dihydrogen phosphate, sodium hydroxide, disodium hydrogen phosphate, potassium dihydrogen phosphate, and ethanol, were procured from Central Drug House (New Delhi, India). For HPLC analysis, double distilled water was filtered through a micron-sized membrane filter (pore size, 0.45µ) and membrane filter (Durapore pore size, 0.21 µ) using an injectable needle.
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8

Cinnarizine-Loaded Lipid Nanoparticles

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Cinnarizine (I.P.) was received from Ray Chemicals (p) Ltd., Bangalore, India. EC (lot no: 02129) was purchased from the Central Drug House (P) Ltd., New Delhi, India, and polyvinyl alcohol (PVA) (lot no: RM 6170) was purchased from Himedia, New Delhi, India. PEG-8 caprylic/capric glycerides (brand name: acconon MC 8-2 EP/NF, Lot no. 090612-8) and glycerol monooleate (brand name: Capmul GMO, Lot no. 100616-8) were obtained from ABITEC Corporation, Janesville, WI, USA. Ethanol (lot no: XK-13-201-00185) and dichloromethane (lot no: R271J06) were obtained from S D Fine-Chem Limited, Mumbai, and Rankem, India, respectively. All other chemicals were procured from local sources and are of high purity.
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9

Quantification of Olmesartan and HCTZ

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Working standards of Olmesartan acid (OLM) and OLM D6 (OLM D6) were procured from VIVAN Life Sciences (Thane-Mumbai, India) and Simson Pharma (Dahisar-Mumbai, India), respectively. Working standard of HCTZ was also procured from VIVAN Life Sciences and HCTZ 13C D2 (HCTZ 13C D2) was purchased from Splendid Lab (Pune, India). OLM D6 and HCTZ 13C D2 were used as internal standards (IS) for OLM and HCTZ, respectively. Methanol was purchased from Merck. Drug-free human plasma with ethylene diamine tetra acetic acid (K2EDTA) was purchased from Laxmi Sai Clinical Labs (Hyderabad, India). Formic acid (SQ grade) and ammonium acetate (Excela R grade) were purchased from Qualigens Fine Chemicals (Mumbai, India). Diethyl ether and dichloromethane were obtained from S.D. Fine Chemicals Ltd. (Mumbai, India). Milli-Q water with resistivity of 8.2 milliohm at 25°C and total organic carbon (TOC) ≤500 ppb was used from the in-house Milli-Q water purifying system (Millipore, SAS, Molsheim, France).
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10

Extraction of Organic Compounds

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An equal volume of dichloromethane (SD Fine Chemicals, Mumbai, India) was added to the sample, poured into a 100 mL separatory funnel and shaken vigorously for 2 min. It was allowed to separate until the solvent and aqueous phases were formed. The solvent phase (dichloromethane) was gently released into a dry test tube. The procedure was repeated twice and the solvent phases were pooled into the test tube and 0.5 g of anhydrous sodium sulphate was added. The test tube was kept for 5 min for the total removal of moisture before transferring the extract into a graduated tube. The extract was concentrated to 500 μL by shaking in a water bath at ambient temperature (Vanaja et al. 2011).
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