dipartimento di biotecnologie molecolari e scienze … · universitÀ degli studi di torino...

UNIVERSITÀ DEGLI STUDI DI TORINO

DIPARTIMENTO DI BIOTECNOLOGIE MOLECOLARI E SCIENZE DELLA SALUTE

Via P. Giuria,5 - 10125 TORINO (ITALIA) Tel. 011/6705240 – 7624 Fax 011/2365241

SUBJECT: Survey on the chemical composition of the VitaMel Food Supplements range using high-performance liquid chromatography interfaced in series with UV-diode array and mass spectrometer spectrophotometer. Experimental part. Dissolution of 10.0 g of sample in 10 mL of a 30/70 solution of water-methanol in order to obtain a complete solubilization. Introduction of 10ul of each product for the chromatographic separation and subsequent qualitative recognition of the active ingredients. The qualitative recognition has been obtained through the acquisition of the UV absorption spectrum in the range of wave lengths between 210 and 420 nm. This has allowed to identify the chemical class membership (polyphenols, caffeic esters, flavans, flavons, flavanols, etc.) and the subsequent confirmation by mass spectrometry through the identification of the molecular weights and of the main fragments. Results are provided in the following pages, these are the chromatograms obtained in UV together with a list of identified substances. In most cases, these substances are not usually encountered in honey and these substances are clearly from vegetable origin. For further confirmation, in products where there was a commonality in the plants used, the results in the respective chromatograms highlight were overlaps to show the substantial commonality in the chromatographic profile. The Analysis Manager

Prof. Claudio Baiocchi




LIFE-MEL

GINSENG SIBERIANO, ECHINACEA PURPUREA, UNCARIA TOMENTOSA, VACCINIUM MYRTILLUS, URTICA DIOICA, TARAXACUM OFFICINALIS, FICUS CARICA, TRIFOLIUM PRATENSE, MORUS ALBA, CICHORIUM INTYBUS, BETA VULGARIS CICLA, INULA HELENIUM, RIBES NIGRUM, MELISSA OFFICINALIS, CALENDULA OFFICINALIS, AVENA SATIVA

min10 20 30 40 50

mAU

0

200

400

600

800

1000

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LIFE_MEL_SOXLHET_NEG.D)

Figura 1: cromatogramma UV acquisito a λ=320 nm

RT IDENTIFIED SUBSTANCES 6.17 POLIFENOLO (DERIVATO ACIDO BENZOICO)

9 POLIFENOLO (DERIVATO ACIDO BENZOICO) 19.9 POLIFENOLO (DERIVATO ACIDO BENZOICO) 26.3 ESTERE DELL’ACIDO CAFFEICO 27.5 POLIFENOLO (DERIVATO ACIDO BENZOICO)

The Analysis Manager Prof. Claudio Baiocchi




LADY-MEL NIGHT TRIFOLIUM PRATENSE, MEDICAGO SATIVA, VITEX AGNUS-CASTUS, MATRICARIA RECUTITA, PASSIFLORA INCARNATA, HUMULUS LUPULUS, VERBENA OFFICINALIS

min5 10 15 20 25 30 35 40

mAU

0

50

100

150

200

250

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350

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LADY_MEL_N_MEOH_H20_NEG.D)


RT IDENTIFIED SUBSTANCES

6.12 POLIFENOLO (DERIVATO ACIDO BENZOICO) 17.7 POLIFENOLO (DERIVATO ACIDO BENZOICO) 23.4 APIGENINA C GLICOSILATA (IN 6 E 8) 26.0 LUTEOLINA-2-GLUCURONIDE 27.5 QUERCETINA-ARABINOSIDE-GLUCOSIDE 29.1 LUTEOLINA-RUTINOSIDE 30.1 LUTEOLINA-GLUCURONIDE-GLUCOSIDE 31.5 RUTINA 31.7 APIGENINA-RUTINOSIDE 33.1 APIGENINA-GLUCURONIDE-ARABINOSIDE 33.3 IRIGENINA 38.4 LUTEOLINA





LADY-MEL DAY TRIFOLIUM PRATENSE, MEDICAGO SATIVA, VITEX AGNUS-CASTUS, MATRICARIA RECUTITA, CALENDULA OFFICINALIS, GINSENG SIBERIANO, MENTHA X PIPERITA OFFICINALIS, SERENOA REPENS

min5 10 15 20 25 30 35 40

mAU

0

50

100

150

200

250

300

350

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LADY_MEL_D_MEOH_H20_NEG.D)



6.08 POLIFENOLO (DERIVATO ACIDO BENZOICO) 17.66 POLIFENOLO (DERIVATO ACIDO BENZOICO) 23.4 APIGENINA C GLICOSILATA (IN 6 E 8) 27.5 QUERCETINA-ARABINOSIDE-GLUCOSIDE 29.1 LUTEOLINA-RUTINOSIDE 30.1 LUTEOLINA-GLUCURONIDE-GLUCOSIDE 31.5 RUTINA 31.7 APIGENINA-RUTINOSIDE 33.1 APIGENINA-GLUCURONIDE-ARABINOSIDE 33.3 IRIGENINA 38.4 LUTEOLINA

min10 20 30 40 50

mAU

50

100

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*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LADY_MEL_D_MEOH_H20_NEG.D)*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LADY_MEL_N_MEOH_H20_NEG.D)

Figura 4: confronto dei cromatogrammi UV acquisiti a λ=320 nm dei campioni LADY-MEL DAY e LADY-MEL NIGHT




RELAX-MEL INULA HELENIUM, AVENA SATIVA, VITEX AGNUS-CASTUS, PASSIFLORA INCARNATA, LAVANDULA ANGUSTIFOLIA, HUMULUS LUPULUS

min10 20 30 40 50

mAU

0

20

40

60

80

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\RELAX_MEL_MEOH_H20_NEG.D)



6.09 POLIFENOLO (DERIVATO ACIDO BENZOICO) 17.67 POLIFENOLO (DERIVATO ACIDO BENZOICO)

20 ESTERE DELL’ACIDO CAFFEICO 21.1 ESTERE DELL’ACIDO CAFFEICO 21.7 ESTERE DELL’ACIDO CAFFEICO 23.4 APIGENINA C GLICOSILATA (IN 6 E 8) 26.0 LUTEOLINA=2GLUCURONIDE 26.5 ESTERE DELL’ACIDO CAFFEICO 29.7 CRISINA-RUTINOSIDE 33.3 IRIGENINA 34.3 FLAVONOIDE 38.4 LUTEOLINA





DEFENCE-MEL GINSENG SIBERIANO, ECHINACEA PURPUREA, UNCARIA TOMENTOSA, BETA VULGARIS CICLA, MEDICAGO SATIVA, SAMBUCUS NIGRA, ECHINACEA PALLIDA, POLYGONUM AVICULARE, ECHINACEA ANGUSTIFOLIA

min5 10 15 20 25 30 35 40

mAU

0

20

40

60

80

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\DEFENCE_MEOH_H2O_NEG.D)



5.46 POLIFENOLO (DERIVATO ACIDO BENZOICO) 6.28 POLIFENOLO (DERIVATO ACIDO BENZOICO) 20 ESTERE DELL’ACIDO CAFFEICO

21.1 ESTERE DELL’ACIDO CAFFEICO 21.7 ESTERE DELL’ACIDO CAFFEICO 26.5 ESTERE DELL’ACIDO CAFFEICO





INFLU-MEL GINSENG SIBERIANO, ECHINACEA PURPUREA, UNCARIA TOMENTOSA, BETA VULGARIS CICLA, MEDICAGO SATIVA, SAMBUCUS NIGRA, ECHINACEA PALLIDA

min5 10 15 20 25 30 35 40

mAU

0

20

40

60

80

100

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\VIR_MEL_MEOH_H20_NEG.D)



4.88 POLIFENOLO (DERIVATO ACIDO BENZOICO) 6.12 POLIFENOLO (DERIVATO ACIDO BENZOICO) 8.99 POLIFENOLO (DERIVATO ACIDO BENZOICO) 20 ESTERE DELL’ACIDO CAFFEICO

21.1 ESTERE DELL’ACIDO CAFFEICO 21.7 ESTERE DELL’ACIDO CAFFEICO 26.5 ESTERE DELL’ACIDO CAFFEICO 33.3 IRIGENINA

min5 10 15 20 25 30 35 40 45

mAU

20

40

60

80

100

120

*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\DEFENCE_MEOH_H2O_NEG.D)*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\VIR_MEL_MEOH_H20_NEG.D)

Figura 8: confronto dei cromatogrammi UV acquisiti a λ=320 nm dei campioni DEFENCE-MEL e INFLU-MEL




POTENT-MEL GINSENG SIBERIANO, INULA HELENIUM, ANGELICA ATROPURPUREA, ARALIA RACEMOSA, VITEX AGNUS-CASTUS, SCHISANDRA CHINENSIS, PANAX GINSENG, SERENOA REPENS, PLANTAGO IMPORTANTI, LEPIDIUM MEYENII, TRIBULUS TERRESTRIS, VITIS VINIFERA

min5 10 15 20 25 30 35 40 45

mAU

0

50

100

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250

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\POTENT_MEL_MEOH_H20_NEG.D)




21.1 ESTERE DELL’ACIDO CAFFEICO





ENERGY-MEL GINSENG SIBERIANO, INULA HELENIUM, ARALIA RACEMOSA, PLANTAGO MAJOR, ANGELICA ATROPURPUREA, VITEX AGNUS-CASTUS, SCHISANDRA CHINENSIS, PANAX GINSENG

min5 10 15 20 25 30 35 40 45

mAU

0

20

40

60

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100

120

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\ENERGY_MEL_MEOH_H2O_NEG.D)




21.1 ESTERE DELL’ACIDO CAFFEICO 33.3 IRIGENINA

min5 10 15 20 25 30 35 40 45

mAU

50

100

150

200

250

*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\POTENT_MEL_MEOH_H20_NEG.D)*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\ENERGY_MEL_MEOH_H2O_NEG.D)

Figura 11: confronto dei cromatogrammi UV acquisiti a λ=320 nm dei campioni POTENT-MEL e ENERGY-MEL




GASTRO-MEL LAURUS NOBILIS, SALVIA OFFICINALI, ANGELICA ATROPURPUREA, HYDRANGEA ARBORESCENS, OPUNTIA FICUS-INDICA, MEDICAGO SATIVA

min10 20 30 40 50 60 70 80

mAU

0

200

400

600

800

1000

1200

1400

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\GASTRO_MEL_MEOH_H20_NEG.D)


RT IDENTIFIED SUBSTANCES 6.1 POLIFENOLO (DERIVATO ACIDO BENZOICO)

17.83 POLIFENOLO (DERIVATO ACIDO BENZOICO) 21.7 ESTERE DELL’ACIDO CAFFEICO 26.5 ESTERE DELL’ACIDO CAFFEICO 29.2 ESTERE DELL’ACIDO CAFFEICO 34.9 ESTERE DELL’ACIDO CAFFEICO 38.4 LUTEOLINA 42.8 FLAVANO 51.3 ESTERE DELL’ACIDO CAFFEICO 52 CRISINA

53.2 PINOCEMBRINA 53.6 GALANGINA 64.1 PINOSTROBINA





CLEAR-MEL PLANTAGO MAJOR, SAMBUCUS NIGRA, POLYGONUM AVICULARE, PINUS SYLVESTRIS, PORTULACA OLERACEA

min5 10 15 20 25 30 35 40

mAU

0

50

100

150

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300

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\CLEAR_MEL_MEOH_H20_NEG.D)


min20 25 30 35 40 45

mAU

0

10

20

30

40

50

60

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\CLEAR_MEL_MEOH_H20_NEG.D)



4.48 POLIFENOLO (DERIVATO ACIDO BENZOICO) 23.4 APIGENINA C GLICOSILATA (IN 6 E 8) 33.3 IRIGENINA 35.6 ESTERE DELL’ACIDO CAFFEICO 38.4 LUTEOLINA





LARINGO-MEL

BETA VULGARIS CICLA, MELISSA OFFICINALIS, CALENDULA OFFICINALIS, LAURUS NOBILIS, SAMBUCUS NIGRA, ORIGANUM MAJORANA, FOENICULUM VOLGARE

min5 10 15 20 25 30 35 40 45

mAU

0

50

100

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350

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LARYNGO_MEL_MEOH_H20_NEG.D)



4.48 POLIFENOLO (DERIVATO ACIDO BENZOICO) 6.14 POLIFENOLO (DERIVATO ACIDO BENZOICO) 23.4 APIGENINA C GLICOSILATA (IN 6 E 8) 33.3 IRIGENINA 35.6 ESTERE DELL’ACIDO CAFFEICO 38.4 LUTEOLINA

min5 10 15 20 25 30 35 40 45

mAU

50

100

150

200

250

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350

*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\CLEAR_MEL_MEOH_H20_NEG.D)*DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\LARYNGO_MEL_MEOH_H20_NEG.D)

Figura 16: confronto dei cromatogrammi UV acquisiti a λ=320 nm dei campioni CLEAR-MEL e LARYNGO-MEL




BRONCO-MEL LAURUS NOBILIS, SALVIA OFFICINALIS, PLANTAGO MAJOR, SAMBUCUS NIGRA, MATRICARIA RECUTITA, EUCALYPTUS GLOBULUS, ROSMARINUS OFFICINALIS

min5 10 15 20 25 30 35 40 45

mAU

0

20

40

60

80

100

120

140

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\BRONCHO_MEOH_H20_NEG.D)


RT IDENTIFIED SUBSTANCES 4.5 POLIFENOLO (DERIVATO ACIDO BENZOICO) 6.01 POLIFENOLO (DERIVATO ACIDO BENZOICO) 8.99 POLIFENOLO (DERIVATO ACIDO BENZOICO) 20 ESTERE DELL’ACIDO CAFFEICO

21.1 ESTERE DELL’ACIDO CAFFEICO 21.7 ESTERE DELL’ACIDO CAFFEICO 23.4 APIGENINA-C-GLICOSILATA (IN 6 E 8) 26.5 ESTERE DELL’ACIDO CAFFEICO 33.3 IRIGENINA 35.6 ESTERE DELL’ACIDO CAFFEICO 38.4 LUTEOLINA





MAG-MEL BETA VULGARIS CICLA, AVENA SATIVA, MEDICAGO SATIVA, PUNICA GRANATUM, JUNGLAS REGIA, PETROSELIUM CRISPUM, PHASEOLUS VULGARIS, CERATONIA SILIQUA

min5 10 15 20 25 30 35 40 45

mAU

0

20

40

60

80

DAD1 B, Sig=320,4 Ref=400,100 (MIELE_ISRAELIANO_NEG_9SET13\MAGNE_MEL_MEOH_H20_NEG.D)



4.88 POLIFENOLO (DERIVATO ACIDO BENZOICO) 6.12 POLIFENOLO (DERIVATO ACIDO BENZOICO) 17.66 POLIFENOLO (DERIVATO ACIDO BENZOICO)

20 ESTERE DELL’ACIDO CAFFEICO 21.1 ESTERE DELL’ACIDO CAFFEICO 21.7 ESTERE DELL’ACIDO CAFFEICO 23.4 APIGENINA C GLICOSILATA (IN 6 E 8) 26.5 ESTERE DELL’ACIDO CAFFEICO 33.3 IRIGENINA 35.6 ESTERE DELL’ACIDO CAFFEICO 38.4 LUTEOLINA


dipartimento di biotecnologie molecolari e scienze … · universitÀ degli studi di torino...

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