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  • Rapid screening of oleuropein from olive leaves using matrix solid-phase dispersion and high-performance liquid chromatography.

Rapid screening of oleuropein from olive leaves using matrix solid-phase dispersion and high-performance liquid chromatography.

Journal of AOAC International (2014-08-26)
Marzieh Rashidipour, Rouhollah Heydari, Alireza Feizbakhsh, Payman Hashemi
ABSTRACT

Matrix solid-phase dispersion (MSPD) methodology as a quick and easy extraction method has been developed to extract oleuropein from Olea europaea leaves. This method has been compared with conventional maceration and Soxhlet extraction (SOXE) methods. Variables affecting MSPD, such as the sorbent material, the ratio of sample to sorbent material, elution solvent, and volume of the elution solvent, have been fully evaluated and optimized. Oleuropein was successfully extracted by silica sorbent with 350 microL of dichloromethane-methanol (70 + 30, v/v) as the elution solvent. The calibration curve showed good linearity (r2 = 0.9985) and precision (RSD <4.5%) in the concentration range of 0.5-100 microg/mL for oleuropein. The LOD and LOQ were 0.14 and 0.5 microg/mL, respectively. The recoveries were in the range of 88.0-94.0% with RSD values ranging from 6.0 to 9.8%. The extraction yields obtained by the MSPD method were comparable with those obtained by the maceration and SOXE methods. The reported MSPD extraction method was revealed to be eco-friendly, simpler, and faster than conventional methods used to quantify oleuropein in O. europaea leaves.

MATERIALS
Product Number
Brand
Product Description

Supelco
Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Oleuropein, ≥80% (HPLC)
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Methanol-12C, 99.95 atom % 12C
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L-Lysine monohydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
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Oleuropein, ≥98.0%
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L-Lysine monohydrochloride, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Ethyl acetate, natural, ≥99%, FCC, FG
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Ethyl acetate, ≥99%, FCC, FG
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Ethyl acetate, ReagentPlus®, ≥99.8%
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Oleuropein, analytical standard
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Acetonitrile, electronic grade, 99.999% trace metals basis
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Ethanol, purum, secunda spirit, denaturated with 2% 2-butanone, S15, ~96% (based on denaturant-free substance)
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Dichloromethane, Selectophore, ≥99.5%
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Hexane, analytical standard
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L-Lysine monohydrochloride, reagent grade, ≥98% (HPLC)
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L-Lysine monohydrochloride, from non-animal source, meets EP, JP, USP testing specifications, suitable for cell culture, 98.5-101.0%
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Ethyl alcohol, Pure, 160 proof, Excise Tax-free, Permit for use required
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
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Acetonitrile, ReagentPlus®, 99%
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Ethyl acetate, ACS reagent, ≥99.5%
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Ethanol, purum, fine spirit, denaturated with 4.8% methanol, F25 METHYL1, ~96% (based on denaturant-free substance)
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Ethanol, purum, absolute ethanol, denaturated with 2% 2-butanone, A15 MEK1, ≥99.8% (based on denaturant-free substance)
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Ultrapure Acetonitrile
Oleuropein, European Pharmacopoeia (EP) Reference Standard
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Ethyl acetate, biotech. grade, ≥99.8%
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Methylene Chloride, Pharmaceutical Secondary Standard; Certified Reference Material