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Physicochemical properties, composition and pollen spectrum of ling heather (Calluna vulgaris (L) Hull)
honey produced in Spain
J Serra Bonvehí, E Granados Tarrés
To cite this version:
J Serra Bonvehí, E Granados Tarrés. Physicochemical properties, composition and pollen spectrum of
ling heather (Calluna vulgaris (L) Hull) honey produced in Spain. Apidologie, Springer Verlag, 1993,
24 (6), pp.586-596. �hal-00891133�
Original article
Physicochemical properties, composition
and pollen spectrum of ling heather
(Calluna vulgaris (L) Hull) honey produced in Spain
J Serra Bonvehí E Granados Tarrés
1 Research
Department, Nutrexpa,
SA and Mielso, SA,Lepanto,
410-414, 08025 Barcelona;2
IRTA,
Centre de Cabrils, 08348 Cabrils, Barcelona,Spain
(Received
6 December 1991;accepted
7 June 1993)Summary —
Thepalynological
andphysicochemical properties
of 28samples
ofcommercially
pro- ducedSpanish ling
heatherhoney
were defined. On the basis of themelissopalynological analysis,
5
samples
were excluded asthey
were of different botanicalorigin;
101 differentpollen
types were identified in theremaining samples.
The relative richness ofpollen
from Calluna was between 10- 33%. Thehigh
incidence of Erica spppollen (usually > 10%),
makesling
heatherhoney
characteri- zation difficult. The sugar spectrum showed low percentages ofglucose
(25.6g/100 g), high
levelsof disaccharides, and traces of sucrose and trisaccharides.
Enzymatic activity
washigher (51.89
units on the Gothe
scale)
than that found in other unifloralSpanish honeys.
The totalacidity
(45.5meq/kg)
exceeds thelegal
limit established forhoney
in the EEC. The mineral elements show a pre- dominance ofpotassium,
sodium and calcium. The differentfluidity
curves were determinedusing
a4-speed (16,
40, 80 and 160 rpm) concentriccylinder
rotary viscometer. Thethixotropical
behaviourof this
honey
was determined as the crumbling index at the maximumtangential
tension that couldbe
generated by
the viscometer used.honey
/ Callunavulgaris / pollen analysis / physicochemical properties / Spain
INTRODUCTION
Although
Calluna is foundthroughout
theIberian
peninsula,
it isbasically predomi-
nant in the area where the
provinces
of Soria and LaRioja
meet. There are alsothe heathers Erica
aragonensis Wilk,
Ericavagans
L,
Ericascoparia
L and Erica ar-borea L
spread extensively
over the Ibero- Sorianhighlands
at the NE limit of thecentral
plateau.
Thesehighlands
consistof the
typical European
transitional scrub-land,
where Erica arborea appears next to Ericascoparia, growing together
with themaquis type comprising Arbutus, Cistus,
* Present address: Laboratori
Agrari (Generalitat
deCatalunya),
Ctra de Cabrils, s/n, 08348 Cabrils(Barcelona), Spain.
Genista, Buxus, Viburnum, Lavandula, Ulex, Myrtus, Thymus,
elements of Quer- cetumsessiflorae, Quercetum
tozaeand,
in certain cases, Quercetum
ilicis,
and inwhich Calluna features as a
principal
char-acteristic
(Tarazona Lafarga, 1984;
Serra Bonvehí and MundoElias, 1988).
Thesecommunities have the
following
character-istics:
they
are veryfrugal,
siliceous andacidulous, they
are welladapted
to thepoor soil conditions of the Ibero-Sorian
Highlands,
and to a climate which is notespecially
prone todrought
or extremetemperatures.
In this area, there are someenclaves where Calluna is
predominant, although
the other heathers do reappear withvarying frequency.
Therefore it is in-teresting
to determine thepollen spectrum
and examine the influence of the presence of Erica spp on Callunahoney,
becausethey
have the sameflowering period.
There are
only
a fewpublished
studies onthe
composition
and characteristic fea- tures ofling
heather and heatherhoney.
Of
these,
the mostimportant
are the stud-ies
by Pryce-Jones (1936; 1944; 1952;
1953),
Louveaux(1966, 1977),
Pourtallier and Taliercio(1970),
Fitó andRodriguez (1981), Spettoli
et al(1982),
Henderson(1984),
Accorti et al(1986), Speer
andMontag (1986),
Persano Oddo et al(1988),
and Tan et al(1989), although they only
determine a few characteristic features. Most of these studies make note of the fact thatling
heatherhoney
hasthixotropical properties,
which make its ex-traction
by centrifugation impossible.
Hence,
the need to use a "loosener" onthe combs. This
study attemps
to be morecomplete,
inthat, apart
from thepollen spectrum,
we determine the most common features of thehoney,
such as: water con-tent; colour;
electricalconductivity;
sugarspectrum;
mineralelements; hydroxy- methylfurfural; enzymatic activity;
true pro-tein
content; viscosity;
andcrumbling
in-dex of the
thixotropical
structure.MATERIAL AND METHODS
Twenty-eight samples
ofcommercially produced ling
heatherhoney
were taken over 2 succes-sive years from the stores of 2 commercial entities; 5 of the
samples
wererejected
on thebasis of
pollen spectra.
Allsamples
came fromlots destined for sale on the market, and had been collected in 1985 and 1986 in the area
where the
provinces
of Soria and LaRioja
meet(Spain).
For each of thesamples,
aquestion-
naire was filled in with data about its
handling by
the
producer,
extraction date, type of bee-hive and nomadic route. Thesamples
were pre- served at 0-5°C in acold-storage
room andanalysed
as soon asthey
arrived in the laborato- ry.Melissopalynological analysis
The
analysis
was carried out in accordance with the methods of the International Commission of BeeBotany (ICBB)
of the International Union ofBiological
Sciences(IUBS),
describedby
Lou-veaux et al
(1978).
Thegrain
count was per- formedfollowing
the methodsuggested by Vergeron (1964)
(1 200grains counted).
The
pollens
identified were classified accord-ing
to theirfrequency.
There were 4 classes ofpollen: predominant
(>45%)
= D;secondary
(16-45%) = S;important
minor (3-15%) = s; mi-nor (< 3%) = r. For the absolute number of pol- len grains, there are 5 groups: group I =
honeys
low in
pollen (PK/10 g
< 20 000); group II = nor- malhoneys (PK/10 g 20 000-100 000);
group III= honeys
rich inpollen (PK/10
g 100 000- 500 000); group IV =honeys extremely
rich inpollen (PK/10
g 500 000-1 000000);
group V =pressed honeys (PK/10 g
> 1 000 000).Physical
and chemicalanalysis
The sugar spectrum was determined in accor-
dance with Serra Bonvehí and Bosch Callis
(1988),
on aSigma
2 gaschromatograph
andquantified
on aSigma
15(Perkin-Elmer)
micro-processor.
The electrical
conductivity
was measured in asolution at 20%
dry weight
and 20°C, in a Crisonmodel 332 conductimeter,
using
continuous flow immersion cells.The
enzymatic activity
followed the method of White and Pairent(1959),
establishedby
theAOAC
(1980),
on a 260 Shimadzu UV-visiblespectrophotometer
at 660 nm.Humidity
was determinedfollowing Chataway (1932)
and Wedmore(1955),
a method estab- lishedby
the FAO/WHO(1969).
We used anAtago
model 8326Abbe-type
refractometer.The colour was determined
using tristimulary methodology (Aubert
and Gonnet, 1983) on a 260 Shimadzu UV-visiblespectrophotometer
with a
path-length
of 1 cm.The free and lactone
acidity
was evaluatedby
the method of White et al
(1958),
and thepH
wasmeasured in a 10% solution in an
Expandable
ionAnalyzer
EA 920(Crion Research) pH-metre.
The
activity
of water in thehoney (a w )
wasdetermined via a Humidat-IC
(Novasina) hy-
grometer at 20 ± 0.5°C.The
nitrogen
content(protein
+ amino acids)was measured
according
to White et al(1962)
on a Bloc
Digest using
a Dosi-Gen S-511(Se- lecta) (N
x 6.25) automatic distiller.Hydroxy- methylfurfural
was determinedby
the method of White(1979).
To determine mineral elements, 5
g honey
was reduced to ashes at 500-550°C and dis- solved in 2 ml and 2 N HCl, made up to 50 ml with distilled water at 40°C, and
Cl 3 La
and CICswere added
(Sanui
and Pace, 1968; DeRuig, 1986).
The K, Na,Mg,
Ca, Fe, Zn, Cr, Cu and Pb contents were evaluatedusing
a model 703atomic
absorption spectrophotometer (Perkin- Elmer).
Pb was determined in 15 ghoney/25
mldistilled water.
The
viscosity
of thehoney
at 20-20.5°C wasdetermined
using
a 4-speed (16, 40, 80 and160 rpm)
concentriccylinder
rotary viscometer, type Searle-Couette, model RN, VEB-MLW, Prüfärate, WerkMedingen (Germany).
The RNmeasuring
mechanism consisted of a bell-shaped
rotor and a innercylinder
inside a meas-uring glass,
both of whichprovide
2shearing
surfaces
(rotor
diameter, 8.57 mm;glass
diame- ter, 15mm).
First thespeeds
of deformation(§, s
-1
)
were calculated, and, with the results read from the scale on the viscometer, shear stress(
þ, dynes/cm 2 )
andapparent viscosity (n, cP)
were determined. The results are
represented graphically by
a system of cartesian coordinates(þ,§)
toyield
thefluidity
curve, from which it ispossible
to work out anequation
that describes therheological
behaviour of the fluid understudy (Prentice, 1984).
The ascendent and de- scendent values weregradually
obtainedby
var-ying
the rotationspeed
of thecylinder
from thehighest
to the lowest, and vice-versa.During
thedeformation
speed
test, values were taken eve-ry 20 s, with the aim of
seeing
the variation that the apparentviscosity
underwentthroughout
thetesting
time. With these values, one can deter- mine thecrumbling
index of thethixotropic
struc-ture
(B) (De
Kée and Turcotte, 1980). For the cal- culation of(B),
thefollowing
formula was used:RESULTS AND DISCUSSION
Table I shows data from the
pollen analy- sis,
and tables II-Vgive
values of chemical andphysical parameters
for the characteri-zation,
andprovide
estimates of their vari-ability.
Five of the 28
samples
studied were re-jected
becausethey presented
a differentbotanic
origin, being
considered multiflow-er
honey
in which there was apredomi-
nance of Erica spp, Centaurea cyanus, Vi- cia sp and
Eucalyptus
sp.In the 23
samples accepted
101 differ- entpollen types
were identified with an av-erage of 40 per
sample,
which exceeds that of theprinciple
monofloralSpanish
honeys (table I) (Serra
Bonvehi etal, 1987;
SerraBonvehí, 1988;
Serra Bonvehí and CañasLloria, 1988).
About half of thesamples (52%)
had a minimum of 39 tax-ons and 30% had less than 37 taxons.
Most of the
samples belonged
to groups III(52%)
and IV(43%) (table I).
Thepercent-
age of Calluna
pollen
was nothigh (X
=17%),
withonly
13% of thesamples being
over 25%. As shown in table
I,
52% of theaccepted samples
contain 16-33% Ericaspp
(X = 24%);
in the rest of thesamples
the presence varies from 2 to 16%
(X
=8%). Unfortunately,
thishigh
Erica spp content makes it difficult toidentify ling
heather
honey through
amelissopalyno- logical analysis. According
to Accorti et al(1986)
heatherhoneys
should contain 45% Erica spppollen
as a minimum. Un-der these
circumstances,
theonly
feasiblealternative is to limit its presence to such a value that its interactions do not
modify
thephysicochemical
characteristics ofling
heather
honey. Approximately
50% of theidentified taxons appear in forms as
impor-
tant minor
(s)
and minorpollen (r).
As dom-inant
pollen (D), only Eucalyptus
sp wasdetected,
with Callunavulgaris
and Ericaspp as
secondary (S). Onobrychis
viciifoliaand
Medicago
sativa stand out among the forms ofpollen belonging
to cultivatedplants.
Four taxons wereoutstanding
intheir different
frequencies (Eucalyptus
sp, Citrus sp, Helianthus annuus and Echiumsp) although they
do notbelong
to thephy- tosociological
communities of the collection area,appearing
as floral remains from otherzones in
Spain
that find their way to Callu-na.
Among
the most characteristic forms identified in thishoney
werespontaneous
and
subspontaneous
adventitiousplants, coming
from other crops such as Ranuncu-laceae,
Umbelliferae andRumexsp.
Pollen forms that were not identified with
certainty
asbelonging
to aparticular
species
or genus weregrouped
underwhat appear to be the most
frequent
forms(type Achillea, type Carduus, type
C(Cen-
taurea
cyanus), type
H(Helianthus
an-nuus), type
R22-25 μ (Brassica sp),
orper group
(Prunus Gr, Pyrus Gr).
The taxons most
frequently
detected inat least 50% of the
samples
were: Callunavulgaris (100%);
Erica spp(Erica
aragonen-sis,
Erica vagans, Ericascoparia) (100%);
Quercus sp
(100%);
Salix sp(100%);
Ru- bus ulmifolius(100%);
Cistus sp(96%);
Cruciferae
type
R22-25 μ (Brassica sp) (96%); Hypecoum
imberbe(96%); Thymus
sp
(96%);
Trifolium repens(96%);
Lavandu-la sp
(96%);
Melitotus sp(91 %); type
Cam-panula (78%); Ligustrum
sp(78%); type
Ge- nista(78%);
Lotus sp(78%); Onobrychis
viciifolia
(78%);
Centaurea cyanus(74%);
Prunus Gr
(74%);
Helianthemum sp(70%);
type
Carduus(65%);
Taraxacum officinale(61 %); Hypericum
sp(61 %);
Satureia mon-tana
(57%); type
Vicia(57%);
and Castaneasativa
(48%).
All theplants
detected werealso
nectariferous,
withexception
ofCaryo- phyllaceae,
Quercus sp,Cistaceae,
Pina-ceae,
Cupressaceae, Gramineae, Papaver rhoeas, Rumex sp
and Ulmaceae.As table II
shows, ling
heatherhoney presented
lowerpercentages
ofglucose,
similar to
fructose, isomaltose, kojibiose
and
melibiose,
with the presence of mal- tosestanding
out assignificantly
different(P = 0.01)
from other unifloralhoneys (Es- pada Herrero, 1984;
Accorti etal, 1986;
Serra Bonvehi
et al, 1987;
SerraBonvehi, 1988; Bogdanov
andBaumann, 1988;
Ser-ra Bonvehí and Cañas
Lloria, 1988;
Saba-tini et
al, 1989).
Thetrisaccharide,
sucroseand F/G index results coincide with find-
ings
of Pourtallier and Taliercio(1970)
andMateo Castro and Bosch
Reig (1984).
The F/G index and therespective
interval(1.29-1.51)
allow for a clear differentiation from Erica spphoney
0.95-1.29(Espada
Herrero, 1984);
0.95-1.25(Accorti
etal,
1986);
0.99-1.25(Sabatini et al, 1989).
The electrical
conductivity
gave an av- erage value of 8.13 x10 -4 S·cm -1 , placing
it between flower
honey
andhoneydew,
asreported by
Pourtallier and Taliercio(1970) (table III).
Ling
heatherhoney presented high
lev-els of diastasic
activity,
withonly
13% ofthe
samples giving
values of less than 40 Gothe units.However,
as heatherhoneys
have low levels of diastasic
activity,
withaverage values recorded at about 10 Gothe units
(Accorti
etal, 1986),
it couldbe
possible
for thisparameter
to be usedas a
differentiating
element between the 2honeys.
The average water content value came out at 17.40%.
However,
43% of the sam-ples
hadhumidity
values over 19%. Thesamples
collected in 1985 had an averagehumidity
of 15.70%. The same was not true forsamples
of year1986,
which re-flected an average content of
19.31%,
which we attribute to different climatic con-ditions
prevailing
in the 2 years of collec- tion. The colour was very similar to Erica spphoney
and thehoneydew
of Quercussp
(Rodriguez López, 1983;
Accorti etal, 1986), having
an average value ofX
=0.55
(table III),
whichcorresponds
to theresults of Aubert and Gonnet
(1983).
There were no indications of fermentation in any of the
samples,
and the values ofactivity
of water(a w )
were less than 0.70(table II),
which makes thegrowth
ofyeasts impossible (Alcalá Aiguilera, 1977).
The results in table III evidence the exis- tence of
high acidities, exceeding
thelegal
limits
(Boe, 1983).
These values are es-sentially
consequences of thepercentages
of
gluconic
acid andgluconolactone
whichmay be
present
in thehoney (Hadorn
andZürcher, 1963).
ThepH
values are similarto those detected
by
Pourtallier and Talier- cio(1970).
The N x 6.25 content oscillates between 0.50 and1.10%,
with an average content of 0.68%(table III),
whichclearly
differentiates the
samples
from the 5 re-fused
samples
and ingeneral
from otherhoneys,
whichpresent
average values of 0.17%(White
etal, 1962).
Thehydroxy- methylfurfural
values obtained(HMF)
aretypical
ofunprocessed honeys,
withonly
6samples (26%) giving
valueshigher
than10 ppm.
Ashing
gave an average mineral con- tent of0.45%,
which is similar to other heatherhoneys (Espada Herrero, 1984;
Accorti et
al, 1986).
The presence of 9 chemical elements was determined(table III),
with a netpredominance
of K and Na(77%
of thetotal),
followedby
Ca(16%), Mg, Fe, Cu,
Cr and Zn. Withrespect
toother unifloral
honeys
studied(Serra
Bon-vehi
et al, 1987;
SerraBonvehí, 1988;
Ser-ra Bonvehí and Cañas
Lloria, 1988),
K was detected inlarger proportions,
without be-coming
useful as adifferentiating
element(P
=0.05). Although
mosthoneys
behavelike Newtonian
liquids, ling
heatherhoney
is more like a non-Newtonian
liquid.
If thegradient
of deformation is maintained as constant(§),
thetangential
tension(þ)
andthe
viscosity (n)
diminish with the time(table IV).
Thisphenomenon
is known asthixotropy, which,
inling
heatherhoney,
we may attribute to the presence of
protein (Pryce-Jones, 1953).
Incontrast,
the re-jected samples
did not showthixotropy, demonstrating
a Newtonian behaviour be-tween
tangential tension, apparent
viscosi-ty
andmeasuring
time.Passage
from agel-sol-gel stage
wasrelatively rapid.
Hav-ing agitated
thehoney
for 5minutes,
wenoticed a
progressive
decrease in viscosi-ty.
Onceagitation
hadceased,
thehoney
did notcompletely
recover itsgel state,
butbehaved as if it was a non-Newtonian fluid.
So
long
asling
heatherhoney
is not sub-ject
to thermal treatment above 70°C(La-
vie and
Gonnet, 1970), thixotropy
will beone of the best
parameters
for its charac- terization. This may be describedby
a rhe-ogram, so
long
as we fix the variables thatoperate
on the measurements in the fol-lowing
ways:through
theascending
anddescending
curves of therheogram; by
theareas of the
fluidity
curves, in which thethixotropy
isproportional
to the area; andvia the
positioning
of thefluidity
curve. Allof these
require
the use ofexpensive
ap-paratus,
and so we used asimpler
Searle- Couette viscosimeter. The differentfluidity
curves were determined at different
speeds
with different values of(§),
as con-stant
throughout
the measurementstage.
Table IV shows the
apparent
viscosities and theapplied tangential
tensions.Table V illustrates the different values of the
crumbling
index of thethixotropic
struc-ture
(B);
the data obtained is best de- scribedby Burgers
model(Scott-Blair, 1970).
To establish the smallestthixotropic
variation that
ling
heatherhoney
should re-quire,
we determined thecrumbling
indexat the maximum
tangential
tension that could begenerated by
the viscosimeter used(table V).
These data may vary agreat deal,
forexample,
Pourtallier and Ta- liercio(1970)
gave a value of 40cP, by
ap-plying
acylinder
rotationspeed
of 1 rpm.To demonstrate the
thixotropical
behaviourof our
honey,
and thereforetypify
it as auniflower
ling
heatherhoney,
a variation in thecrumbling
index of a minimum of 120 cP at 20-20.5°C was necessary when thecorresponding tangential
tensions were ap-plied
at a rotationspeed
of thecylinder
of160 rpm for 60 s.
Résumé —
Propriétés physicochimi-
ques,composition
etspectre pollinique
du miel de callune
(Calluna vulgaris (L) Hull) produit
enEspagne.
Les caractéris-tiques polliniques
etphysicochimiques
de28 échantillons de miels de callune du
commerce
produits
enEspagne
ont étéétudiées. Sur la base de
l’analyse
mélisso-palynologique (méthodes
del’UISB,
Lou-veaux et
al, 1978),
5 échantillons(18%)
ont été éliminés pour avoir une
origine
bo-tanique
différente. Dans les autres échan-tillons,
101types polliniques
ont été identi-fiés,
avec une moyenne de 40 par échan- tillon(tableau I).
La teneur enpollen
estélevée (100 000
à 500 000 PK/10g).
La ri-chesse relative en
pollen
de Calluna sesitue entre 10 et 33%
(tableau I).
La forteprésence
depollens
du genre Erica(en général > 10%)
rend la caractérisation du miel de callune difficile. Lespectre
des su-cres
présente
de faiblespourcentages
deglucose (25,6 g/100 g),
des teneurs éle- vées en disaccharides et des traces de saccharose et de trisaccharides(tableau II).
L’activitéenzymatique (51,89
unités surl’échelle de
Gothe)
estplus
forte que dans les autres miels monoflorauxespagnols.
L’acidité totale
(45,5 meq/kg) dépasse
la li-mite
légale
établie par la CEE pour les miels. Iln’y
a pas designes
de fermenta- tion et l’activité de l’eau aw est < 0.70.L’analyse
minérale montre uneprédomi-
nance du
potassium,
du sodium et du cal- cium. Les diverses courbes de fluidité ont été déterminées à l’aide d’un viscosimètre rotatif àcylindre concentrique
aux 4 vites-ses suivantes :
16, 40,
80 et 160 rpm(ta-
bleau
IV).
Lecomportement thixotrope
dumiel de callune a été déterminé par l’indice de
désagrégation (crumbling index,
DeKée and
Turcotte, 1980)
calculé à la ten- siontangentielle
maximumproduite
par le viscosimètre utilisé(tableau V).
miel / Calluna /
caractéristique physico- chimique
/analyse pollinique
/Espagne Zusammenfassung —
Zusammenset- zung,physikalisch-chemische Eigen-
schaften und
Pollenspektrum
imspani-
schen
Heidehonig (Calluna vulgaris L).
Pollenspektrum
undphysikalisch-
chemische
Eingeschaften
von 28 Heideho-nigproben
kommerziellerspanischer Honigerzeuger
wurdenanalysiert.
Nachder
melissopalynologischen Analyse (Me-
thodik der
UISB,
Louveaux etal, 1978)
waren 5 Proben abweichender botani- scher Herkunft und wurden
zurückgewie-
sen. In den
übrigen
Proben wurden 101 Pollenartengefunden,
im Durchschnitt ent- hielt eine Probe 40 verschiedene Pollenar- ten(Tabelle I).
DerPollengehalt
war hoch(100 000-500 000
PK/10g).
Der relative Anteil an Calluna Pollenbetrug
zwischen10 und 33%
(Tabelle I),
und der hohe Anteil an Erica spp(>
10% imallgemei- nen)
Pollen stellt ein Problem für die Cha-rakterisierung
dar. DasZuckerspektrum zeigte
hohe Anteile anDisacchariden,
ge-ringen
Gehalt von Glukose(25,6 g/100 g),
und
Spuren
von Saccharose und Trisac- chariden(Tabelle II).
Dieenzymatische
Aktivität
(Gothe-Zahl 51.9)
war höher alsin anderen
spanischen
unifloralen Honi- gen. Der durchschnittlicheSäuregrad (45.5 meq/kg) lag
höher als die von der EEG fürHonig
erlaubten Grenzen. An mi-neralischen Bestandteilen
überwogen
Na-trium-,
Kalium- und Kalziumsalze. Esgab
keineGärungsanzeichen
und die Wasser-aktivität,
aw, war < 0.70. Dasthixotropi-
sche Verhalten wurde mit einem Viskosi- meter bei 4
Umdrehungsgeschwindigkei-
ten
(16, 40,
80 und 160rpm)
desZylinders
charakterisiert
(Tabelle IV, V).
Honig
/ Calluna /physikalisch-
chemische
Eigenschaft
/Pollenanaly-
se
/ Spanien
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