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2 protocols using n butanol

1

Quantitative Analysis of Anticancer Biomarkers

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The three anticancer biomarkers, ursolic acid, β-sitosterol and lupeol were procured from Sigma Aldrich (USA). The solvents used (petroleum ether, ethyl acetate, toluene, chloroform, ethyl acetate, methanol and n-butanol; AR grade) were purchased from BDH (UK). The HPTLC plates (glass-backed silica gel 60F254) were purchased from Merck (Germany). The application of biomarkers and extracts (band wise) to the plate was carried out by Automatic TLC Sampler-4 (CAMAG, Switzerland) while the development took place in automatic development chamber (ADC2, Switzerland). The developed plate was derivatized with p-anisaldehyde reagent [the reagent was prepared according to the Wagner and Bladt (2004) by using anisaldehyde, glacial acetic acid, methanol and concentrated sulphuric acid. Initially anisaldehyde (0.5 mL) was mixed with glacial acetic acid (10 mL) followed by addition of methanol (85 mL) and then sulphuric acid (5 mL)]. The scanning and documentation of developed HPTLC plate was carried out by CATS 4 (CAMAG, Switzerland) and TLC Reprostar 3 (CAMAG, Switzerland), respectively.
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2

Comprehensive Analysis of Organoalkoxysilanes Properties

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The used AS (Table 1) was purchased from Millipore-Sigma, USA. Ethyl acetate, tetrahydrofuran (THF), and ammonium hydroxide were from Sigma-Aldrich, methanol from Lichrosolv, while acetonitrile and n-butanol were from BDH. Dimethyl formamide (DMF), dioxane, and acetic acid were purchased from Riedel-de-Haën, Koch-light laboratory, and Hipersolv, respectively. All the solvents were used without further purification. The water contents were determined using Karl Fischer (KF) reagents (Generator Solution 1613 and Vessel Solutions 1612 from GFS Chemicals, USA). The properties of the used solvents are tabulated in Table 1.

Abbreviations, names, structures and calculated properties (pKa16 (link), partition coefficients18 , α and β values18 , molecular volume (V)17 , and logP17 ) of used OAS.

Organoalkoxysilanes (OAS)pKalogP (water, organic solvent)(α and β of silane)VLogP
AbbreviationName/structureMethanolacetonitrileDioxaneαβ
OTES0.50.81.65.226.22600.28711464.7
CTES0.40.51.22.673.362.880.033

0.275 (O)

0.438 (N)

9082.76
PTES0.11.31.32.713.503.330

0.28 (O)

0.489 (Si)

8873.47
ISBTES001.33.464.153.7800.287(O)8562.95
STES0.90.912.983.943.730.131(S)

0.282(O)

0.235(S)

8953.63
ATES

0.2

N (10)

0.61.60.581.281.010.035(N)

0.285(O)

0.735(N)

8732.12
DMDES−1.1−0.71.821.471.9500.376(O)6282.18
DPDES2.52.64.925.66.200.365(O)9704.91
TMES−2.62.572.452.6500.466(O)5631.97
TEOS0.80.9

1.1

1.2

2.963.23.0900.198(O)7992.25
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