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Separation and purification of sulforaphane from broccoli by solid phase extraction.

Han D, Row KH - Int J Mol Sci (2011)

Bottom Line: The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix.The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1) was 0.02 μg/mL.The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemical Engineering, Inha University, 253 Yonghyun-Dong, Nam-Ku, Incheon 402-751, Korea; E-Mail: hdd_216@hotmail.com.

ABSTRACT
A simple solid-phase extraction (SPE) method for the determination of sulforaphane in broccoli has been developed. The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix. The extracts were sufficiently clean to be directly injected into high-performance liquid chromatography (HPLC) for further chromatographic analysis. Good linearity was obtained from 0.05 to 200 μg/mL (r = 0.998) for sulforaphane with the relative standard deviations less than 3.6%. The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1) was 0.02 μg/mL. The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.

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The molecular structure of sulforaphane in broccoli.
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f1-ijms-12-01854: The molecular structure of sulforaphane in broccoli.

Mentions: Broccoli is a famous vegetable around the world, belonging to the cruciferous family, which is rich in antioxidants such as vitamin C, quercetin and kaempferol [1,2]. Medicinal studies have shown that increasing consumption of broccoli can lower the risk of breast [3], skin [4] and prostate [5] cancers. Recent research showed that glucoraphanin (4-methylsulfinybutyl glucosinolate) is another important constituent in broccoli and it can produces sulforaphane when hydrolyzed by myrosinase. Sulforaphane (Figure 1) has attracted researchers’ attention as a promising cancer chemopreventive agent [6]. In many studies, sulforaphane can reduce the incidence of a number of forms of tumor [7–10]. It is important to develop a rapid and simple method for determination and separation of sulforaphane from broccoli. Several analytical methods such as high-performance liquid chromatography (HPLC) [11,12], GC/mass spectrometry [13] and evaporative light-scattering [14] have been used to determine sulforaphane in broccoli. Meanwhile, preparative HPLC [15] and high-speed countercurrent chromatography [16] have been used to purify sulforaphane. However, the enzymatic hydrolysis of glucoraphanin generates a variety of compounds (glucose, sulfate, isothiocyanates, thiocyanates, nitriles) which interfere with the separation and determination of sulforaphane. Therefore, it is necessary to establish a simple and convenient method for the selective extraction and separation of sulforaphane from broccoli.


Separation and purification of sulforaphane from broccoli by solid phase extraction.

Han D, Row KH - Int J Mol Sci (2011)

The molecular structure of sulforaphane in broccoli.
© Copyright Policy - open-access
Related In: Results  -  Collection

License 1 - License 2
Show All Figures
getmorefigures.php?uid=PMC3111637&req=5

f1-ijms-12-01854: The molecular structure of sulforaphane in broccoli.
Mentions: Broccoli is a famous vegetable around the world, belonging to the cruciferous family, which is rich in antioxidants such as vitamin C, quercetin and kaempferol [1,2]. Medicinal studies have shown that increasing consumption of broccoli can lower the risk of breast [3], skin [4] and prostate [5] cancers. Recent research showed that glucoraphanin (4-methylsulfinybutyl glucosinolate) is another important constituent in broccoli and it can produces sulforaphane when hydrolyzed by myrosinase. Sulforaphane (Figure 1) has attracted researchers’ attention as a promising cancer chemopreventive agent [6]. In many studies, sulforaphane can reduce the incidence of a number of forms of tumor [7–10]. It is important to develop a rapid and simple method for determination and separation of sulforaphane from broccoli. Several analytical methods such as high-performance liquid chromatography (HPLC) [11,12], GC/mass spectrometry [13] and evaporative light-scattering [14] have been used to determine sulforaphane in broccoli. Meanwhile, preparative HPLC [15] and high-speed countercurrent chromatography [16] have been used to purify sulforaphane. However, the enzymatic hydrolysis of glucoraphanin generates a variety of compounds (glucose, sulfate, isothiocyanates, thiocyanates, nitriles) which interfere with the separation and determination of sulforaphane. Therefore, it is necessary to establish a simple and convenient method for the selective extraction and separation of sulforaphane from broccoli.

Bottom Line: The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix.The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1) was 0.02 μg/mL.The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.

View Article: PubMed Central - PubMed

Affiliation: Department of Chemical Engineering, Inha University, 253 Yonghyun-Dong, Nam-Ku, Incheon 402-751, Korea; E-Mail: hdd_216@hotmail.com.

ABSTRACT
A simple solid-phase extraction (SPE) method for the determination of sulforaphane in broccoli has been developed. The optimal conditions were found to be use of a silica SPE cartridge, and ethyl acetate and dichloromethane as washing and eluting solvents, respectively, which could eliminate interferences originating from the broccoli matrix. The extracts were sufficiently clean to be directly injected into high-performance liquid chromatography (HPLC) for further chromatographic analysis. Good linearity was obtained from 0.05 to 200 μg/mL (r = 0.998) for sulforaphane with the relative standard deviations less than 3.6%. The mean recoveries of sulforaphane from broccoli were more than 90.8% and the detection limit (S/N = 3:1) was 0.02 μg/mL. The SPE method provides a higher yield of sulforaphane from crude extracts compared to conventional liquid-liquid extraction.

Show MeSH