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Controlled Release of Fluidized Bed-Coated Menthol

Powder with a Gelatin Coating
a

Pengyu Sun , Maomao Zeng , Zhiyong He , Fang Qin & Professor Jie Chen

State Key Laboratory of Food Science and Technology, School of Food Science and
Technology , Jiangnan University , Wuxi , Jiangsu , China
Published online: 26 Sep 2013.

To cite this article: Pengyu Sun , Maomao Zeng , Zhiyong He , Fang Qin & Professor Jie Chen (2013) Controlled Release
of Fluidized Bed-Coated Menthol Powder with a Gelatin Coating, Drying Technology: An International Journal, 31:13-14,
1619-1626, DOI: 10.1080/07373937.2013.798331
To link to this article: http://dx.doi.org/10.1080/07373937.2013.798331

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Drying Technology, 31: 16191626, 2013

Copyright # 2013 Taylor & Francis Group, LLC
ISSN: 0737-3937 print=1532-2300 online
DOI: 10.1080/07373937.2013.798331

Controlled Release of Fluidized Bed-Coated Menthol

Powder with a Gelatin Coating
Pengyu Sun, Maomao Zeng, Zhiyong He, Fang Qin, and Jie Chen

Downloaded by [Maomao Zeng] at 00:06 28 September 2013

State Key Laboratory of Food Science and Technology, School of Food Science and Technology,
Jiangnan University, Wuxi, Jiangsu, China

We estimated the release properties of uidized bed-coated menthol powder by static headspace analysis and by relating the release
properties and the properties of the coating. Powder was spray-dried
onto different coating materials such as gelatin, an oil-gelatin
emulsion, modied starch, and Aquacoat1 ECD in a uidized bed
system, and then submerged in water at 37
C with a shearing force.
The release properties of encapsulated menthol powder were
estimated over 15 min compared with spray-dried powder. The
microencapsulation efciency of menthol powders was determined,
as well as the density, surface tension, viscosity, and powder contact
angle of coating materials. The gelatin emulsion was found to be a
potential coating material for controlling menthol release from the
coating powder and high microencapsulation efciency (90.44%)
achieved; 60% of the menthol powder was released after 11 min.
These results indicate that the solubility and integrity of the coating
is important to the success of the uidized bed-coating process for
controlled release of avor from this degradation-activated release
system.
Keywords Controlled release; Fluidized bed coating; Menthol;
Static headspace analysis

INTRODUCTION
Menthol, a cyclic terpene alcohol abundant in oils of
peppermint and corn mint, plays an important role in consumer satisfaction and inuences further consumption of
foods, including chewing gum, hard candy, and beverages.
Menthol is normally available in crystalline form with a
melting point of 4143
C. Its stability during storage, an
obvious problem in different foods because of shelf-life
concerns, has been solved by the spray-drying process.
However, it is still difcult for this process to provide controlled delivery of the core material at the desired time and
site.[1] Microencapsulation is a common method to solve
this problem.
Microencapsulation is a process in which tiny particles or
droplets are surrounded by a coating, or embedded in a
homogeneous or heterogeneous matrix. Microencapsulation
Correspondence: Professor Jie Chen, State Key Laboratory of
Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi, Jiangsu 214122, China;
E-mail: chenjie@jiangnan.edu.cn

of avors can be applied to retain aromas in a product during storage, protect the avor from undesirable interactions
with the food, guard against light-induced reactions and=or
oxidation, and allow for controlled release.[2] Techniques
used to form these capsules are classied into three types:
physical processes, chemical processes, and physiochemical
processes. However, toxic agents limit the microencapsulation of avor by physiochemical processes and chemical processes such as coacervation. Physical processes, including
spray drying, spray chilling, extrusion coating, uidized
bed coating, liposome entrapment, inclusion complexation,
and rotational suspension separation, are potential ways
to microencapsulate avor in food.
The most common commercial process to mechanically
encapsulate avors is spray drying, in which a liquid
product is atomized in a hot gas current to instantaneously
form a powder.[3] However, low-boiling point aromatics
can be lost during spray drying; the core avor may also
coat the surface of the capsule, which could cause avor
changes in the product.[4,5] Another problem with spray
drying is that it produces a very ne powder (10100 mm
in diameter) that needs further processing for specic functions such as controlled release.[6] To avoid these problems,
spray-dried powders can be coated using the uidized bed
process.
In uidized bed coating, granules or coated particles are
produced in a single piece of equipment by spraying a
binder in a solution, suspension, or melt onto a uidized
powder bed. Fluidized bed coating is the most suitable
technology for encapsulating spray-dried avors, where
the avors are rst encapsulated by spray drying, because
the wall materials used in avor systems are readily dissolved and form strong inter-particle bridges upon
re-drying.[7] Several researchers have studied the encapsulation of spray-dried powder by uidized bed coating.[811]
However, few papers have reported on the controlled
release properties of avors in capsule matrices.
An enormous range of encapsulating methods can be
used, including proteins, carbohydrates, lipids, gums, and
cellulose, because of the advantage offered by their

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SUN ET AL.

lm-forming ability.[12] The lm-forming ability of a coating material in the uidized bed process is related to its
properties, such as density, surface tension, viscosity, and
powder contact angle. Other than lm-forming ability,
the solvability of the coating material is another signicant
factor related to the release of avor by degradation.
After producing the uidized bed-coated menthol powder, it is important to determine how the avor is perceived
by the taster as it is released in the mouth. Dening the
fraction of the total added avor in the food that is available for perception is difcult. For the same avor experience to be perceived from different food matrices, the same
prole of avor compounds must be received at the avor
receptors in the mouth and nose with the same timing
across all matrices.[13] If this hypothesis is true, then it
should be possible to predict the perceived avor in vivo.
Initially, avors are released from the food to the saliva
phase. Non-volatile avors in saliva are then sensed by
taste buds on the tongue. Volatile avor compounds, however, must be transported from the saliva phase to the air
phase in the mouth, then travel via the throat to the olfactory receptors located in the nose, where they are sensed.[14]
An estimation of the release properties of encapsulated
powder was attempted using static headspace analysis, a
method developed to analyze dynamic volatile release using
gas chromatography.[15]
In this study, gelatin, starch sodium octenyl succinate
(SSOS), and Aquacoat1 ECD (ethyl cellulose aqueous
dispersion) were selected as materials used to coat the
spray-dried menthol powder by the uidized bed process.
The release properties were estimated by static headspace
analysis. Additionally, relationships between the properties
of the coating materials and the release properties were
studied in order to explore the factors that inuence the
controlled release of avor coated by the uidized bed process. Finally, microencapsulation efciency was determined
to ensure a high-quality powder.
MATERIALS AND METHODS
Materials
l-menthol was purchased from Sanhetang Pharmacy
(Guangzhou, China). Starch sodium octenyl succinate
was purchased from Sanfu Food Co., Ltd. (Zhejiang,
China). The modied starch, which was derived from a
waxy maize base, involved the addition of n-octenyl
succinic anhydride (OSA). Gelatin (type A, average molecular weight 110 kDa) was purchased from Sinopharm
Chemical Reagent Co., Ltd. Aquacoat1 ECD was
obtained from FMC (Philadelphia, PA, USA). Triethyl citrate (TEC) and hydroxypropylmethyl cellulose (HPMC)
were purchased from Tiantong Shipinpeiliao Co., Ltd.
(Zhengzhou, China). Food-grade soybean oil was purchased locally. The other organic chemicals used were of
analytical grade.

Preparation of Spray-Dried Powder

The commercial modied starch (i.e., SSOS) was
dispersed in distilled water using a stirrer (RW20.n, IKA,
Germany) at 200 rpm to obtain a 30% w=w wall material
solution, which was rehydrated overnight at room temperature. l-menthol was melted by heating to 60
C; it was
then added to the solution at 60
C to form a melt of 25%
l-menthol (dry basis). The emulsions were homogenized
using a homogenizer (T18 basic, IKA, Germany) at a rotational speed of 17,500 rpm for 3 min; it was further homogenized using a homogenizer (ATS Engineering, Inc.) at
500=150 bar. The emulsions were kept at 60
C and immediately fed to the spray dryer (B-290, BUCHI, Switzerland).
The operational conditions were as follows: inlet temperature: 180
C, outlet temperature: 95  5
C. The nished
powder was stored in a sealed plastic bag at 60
C.
Preparation of Coating Solutions
Gelatin solutions were made of 2%, 5%, 10%, and 15%
gelatin dissolved into distilled water at 60
C. Gelatin emulsions were made of 4% glycerin, 10% gelatin, and some soybean oil. The glycerin and gelatin were dissolved in distilled
water to form a water phase. After adding soybean oil to
5%, 10%, 15%, or 20% weight of gelatin, emulsions were
made as described in the preparation of the spray-drying
feed. The SSOS solution was made of 10% SSOS in distilled
water. The preparation of Aquacoat1 ECD was identical to
that done by Pearnchob and Bodmeier.[16] Aquacoat1 ECD
was plasticized with TEC (25% w=w, based on the polymer)
for 24 h prior to coating. The polymer content of the plasticized dispersion was then adjusted to 15% w=w by dilution
with water; 2% HPMC was added to the solution before
spraying.
Fluidized Bed-Coating Process
One kg of spray-dried powder was coated with 200 mL
of one of the following coating materials: gelatin, gelatin
emulsion, SSOS, or Aquacoat1 ECD. The powder was laid
into the bed, and then hot air was conveyed through the
uidized bed dryer for preheating. After a stabilized uidized bed formed and the inlet temperature rose to 60
C,
one of the coating solutions was delivered onto the powder
bed by a peristaltic pump. The uidized bed parameters
were as follows: coating solution feed rate, 0.2, 0.6,
1.2 mL=s; atomization pressure, 2.0 MPa; outlet temperature, 30
C; inlet temperature, 60
C. The internal operation
was the process in which the coating solution was paused
to spray for 5 min until spraying continued.
Total Oil Measurement
A total of 0.1 g of powder or granules was dispersed in
1 mL of water in a tube with a plug, after which 4 mL of
acetone with methyl salicylate (1 mg  mL1), used as an

FLUIDIZED BED-COATED MENTHOL POWDER

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internal standard, was added, followed by forceful mixing

with a vortex mixer (Genius 3, IKA, Germany) for 1 min.
To extract encapsulated l-menthol into 5 ml of n-hexane,
the mixture was extracted by microwave-auxiliary extraction for 30 min with intermittent shaking. 2 mL of the supernatant was then injected twice for each sample into a gas
chromatograph (GC-2010 Plus, Shimadzu, Japan)
equipped with a 30 m  0.32 mm  0.25 mm glass column
(CP-WAX) and a FID detector. The temperatures of the
detector and the injector were set at 60
C and 250
C,
respectively. The column temperature rose at 10
C  min1
and was constant at 220
C for 3 min. The internal standard
method was used to calculate the amount of menthol. All
of the samples were analyzed in duplicate.
Surface Oil Measurement
A total of 0.2 g of powder was washed in a glass bottle
with 4 ml of n-hexane containing methyl salicylate
(1 mg  mL1) as the internal standard. The mixture was
slowly mixed on a rotary shaker for 30 s at ambient temperature. Once the powder in the mixture had settled, the
menthol content in n-hexane was measured by gas chromatography as described above. The results are the average of
triplicates of each sample.
Calculation of Encapsulation Efficiency
The microencapsulation efciency (ME) was calculated
as follows:
ME Total oil  Nonencapsulatedoil=Total oil  100%
Determination of Coating Material Properties
A dynamic measurement of dynamic viscosity was performed with an AR1000 Rheometer from TA Instruments
(frequency from 102 to 102 Hz and strain from 1 to 100%)
using cone-plate geometry with two 6-cm diameters and an
angle of 4
. The measurements were performed at 60
C.
The linear regime was checked and dynamic experiments
were performed within this linear viscoelastic region. The
density of each coating solution was determined by a densimeter. Tension was determined by an a tensiometer
(DCAT21, Data Physics Instruments GmbH, Filderstadt,
Germany).
Determination of Powder Contact Angle
The apparatus was implemented using a tensiometer
(DCAT21, Data Physics Instruments GmbH, Filderstadt,
Germany). The spray-dried powder was packed into a glass
tube (8  0.1 mm diameter) with a porous glass structure
(glass frit) on its bottom. The tube was mounted on a probe
attached to an electronic balance. A container containing
the test liquid was placed on a moving stage after the
material packing constant C was calculated from the

1621

governing equation using n-hexane. We ensured constant

packing and homogeneous densities across the powder test
samples in order to obtain the best possible reproducibility.
Static Headspace Analysis of Controlled Release
Estimation of the controlled release of the encapsulated
powder was made according to the method of Robert and
Acree.[15] 0.6 g of powder or granules was put into a
120 mL glass bottle with a cap containing a sealed pore
for the injection of 1 mL of headspace. 40 mL of distilled
water at 37
C was added into the bottle, and the cap was
screwed on immediately; meanwhile, timing had already
started. The mixture of powder or granules and water
was stirred in a vortex mixer, and kept at 37
C by a thermostatically controlled water bath (DC10-K10, HAAKE,
Germany). The temperatures of the detector and injector
were set at 80
C and 250
C, respectively. The column temperature rose at a rate of 15
C  min1 and was controlled
at 180
C for 2 min. Samplings of the headspace were
injected manually into a gas chromatography system
(GC-2010 Plus, Shimadzu, Japan) at 1, 3, 5, 7, 9, 11, 13,
and 15 min. To maintain the pressure inside the bottle,
the headspace at every timing point was sampled from
duplicate mixtures.
The accumulative release (AR) was calculated as
follows:
AR A15  Ax =A15   100%
A; peak area; x 1; 3; 5; 7; 9; 11; 13; 15

RESULTS AND DISCUSSION

Fluidized Bed-Coating of Powder
The uidized bed-coating process of spray-dried powder
cannot avoid coating and agglomeration because the size of
the spray-dried powder ranges from 10 to 100 mm. According to Saleh et al.,[17] growth was mainly governed by
layering for particles larger than 200 mm and agglomeration
for smaller particles. After forming the stabilized uidized
bed, the effects of water evaporation from the coating layer
surface on the coating process are signicant; a low evaporation rate caused powder adherence, inducing bed collapse.
Water evaporation is related to the feed ow rate, and the
interval of operation when the air ow rate is xed for a
stabilized uidized bed. Additionally, the temperature cannot be raised beyond a critical value to avoid volatile avor
release.
A series of experiments of uidized bed coatings were
conducted with a 10% gelatin solution as a coating
material. Experimental data presented in Fig. 1A show a
nearly linear increase of accumulative release as a function
of time. However, the curves for different feed ow rates
are difcult to distinguish from each other. This similarity

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SUN ET AL.

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FIG. 1. (A) Effect of feed ow rate on the accumulative release curves over time; (B) effect of internal operation on the accumulative release curves over
time.

indicates that increasing the feed ow rate does not contribute to predominant agglomeration of the particles.
The result agrees with Ichikawa and Fukumoris report.[18]
Compared with Fig. 1A, Fig. 1B shows the same linear
increase. However, it is obvious that internal operation
makes the initial release of two pauses at the timing of
1 min lower than none pause and the release rate is higher.
This result suggests that the integrity of the lm is
improved by halting the feed of the coating solution when
the powder has had enough time to dry water on the
surface. The internal operation produced a multi-layered
coating, which is common in the eld of pharmacy.[19]
Figure 2 shows that different size scales have similar
release curves. This result demonstrates that particle size
contributes to avor release. A description of the agglomeration behavior was explored by Iveson et al.[20] There
may be two reasons: the larger-sized granules composed

FIG. 2. The accumulative release curve of the sample coated with 10%
gelatin solution by two internal pauses after sieving analysis.

of smaller ones were weak and porous, or the larger

granules cannot form a thicker, harder coating bonded
by gelatin as a binder.

Different Materials as the Coating Solutions

The accumulative release curves of four kinds of coatings are presented in Fig. 3. The curve of modied starch
is a gently sloped line with a high release value at 1 min.
Modied starch did not protect initial avor release from
dissolution in water. Merely increasing the coating thickness cannot control avor release in water. Since SSOS is

FIG. 3. The effect of different coating materials on the curve of accumulative release over time. Compositions of the four solutions are as follow:
modied starch, 10% SSOS; gelatin, 15% gelatin; Aquacoat ECD, 25%
TEC based on polymer, 2% HPMC, 15% ECD; emulsion, 20% oil based
on gelatin, 10% gelatin, 4% glycerin. All the samples were coated by the
same coating condition with no pauses.

Downloaded by [Maomao Zeng] at 00:06 28 September 2013

FLUIDIZED BED-COATED MENTHOL POWDER

the wall material used in spray-dried powder, it can help

SSOS coat onto the powder easily.
In contrast, avor release from ECD powder is slow and
uniform. It has a linear curve with no initial release, and
reaches more than 60% for 9 min. According to the different theories of controlled release by Madene,[6] ECD coatings allowed for avor release by diffusion from the core of
the powder to the outside because of the lm-forming ability of insoluble ethyl cellulose. ECD has the best controlled
release behavior among the four coatings; it even overcomes the insolubility of ethyl cellulose as a coating solution. However, it is not the choice for food avor due
to the fact that it contains TEC and other inedible matters.
Gelatin powder sustainably released avor at about a
39% release value after 1 min, and had a greater than
60% release value at 5 min, as presented on its linear curve.
Gelatin has an excellent lm-forming ability and will gel-up
below 40
C. Yoshii[21] added gelatin to maltodextrins and
gum Arabic carrier mixtures to provide better
controlled-release properties, and the results have suggested that gelatin would promote the formation of a crust
on the surface of the droplet. Furthermore, gelatin emulsion provides better controlled-release properties than the
gelatin solution; it had less than a 10% release value at
1 min and more than 60% until 11 min, as shown by
Fig. 3. This result indicates that the addition of oil into
the gelatin solution can improve the protection ability from
water erosion, which agrees with Ma et al.,[22] who added
oil into gelatin to obtain a better edible lm. Addition of
oil may be an effective way to control avor release when
compared with AquaCoat1 ECD.
The microencapsulation efciency of the powder-coated
gelatin emulsion was about 95%, which was the highest of
the four materials presented in Fig. 4. This result indicates

FIG. 4. The effect of different materials on the microencapsulation

efciency. C1: control 1 is spray drying powder; C2: control 2 is powder
through uidized bed process with water as a binder; compositions of
the four solutions are as described above.

1623

FIG. 5. The effect of different gelatin concentrations on the curve of

accumulative release over time. All the samples were coated by the same
coating condition with no pauses.

that material choice affects microencapsulation efciency.

This explanation is illustrated in more detail in the gure
for determination of microencapsulation efciency.
Gelatin/Gelatin Emulsion as the Coating Solution
The solubility of the coating powder inuenced its
release properties, as shown in Fig. 3. The solubility of
the coating powder depends on two factors: coating
material solubility and the integrity of the coating layer.

FIG. 6. The effect of different oil concentrations in gelatin emulsions on

the curve of accumulative release over time. All the samples were coated
by the same coating condition with no pauses.

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FIG. 7. Determination of microencapsulation efciency. (A) The effect of different concentrations of gelatin on the microencapsulation efciency; (B)
the effect of different additions of oil content in emulsion on the microencapsulation efciency; C1: control 1 is spray drying powder; C2: control 2 is
powder through uidized bed process with water as a binder.

The properties of the coating solution inuence the

integrity of the coating layer and the success of the coating
process; the success depends on how the coating droplet
spreads out on the surface of the powder.[23] Several experiments were carried out using coatings made from gelatin
solutions of different concentrations (Fig. 5) and a 10%
gelatin solution with different oil contents (Fig. 6). These
experiments studied the effects of the properties of the
gelatin=gelatin emulsion on avor controlled release.
The measured properties of gelatin=gelatin emulsion
solutions are shown in Table 1. Increasing the gelatin concentration leads to an increase of viscosity and decrease of
surface tension, which contribute to decreasing the powder
contact angle. When additional oil was added to the 10%
gelatin solution, the same property changes occurred.
Kirchberget[24] also found that higher surface tension
would lead to a larger contact angle, which reduced the
droplets wetting capacity. According to Washburns
equation, liquid viscosity changes inversely with a contact
angle, which also improves droplet wetting capacity.
Furthermore, high-pressure homogenizing resulted in the

prominent decline of emulsion viscosity, which explains

the larger contact angle in the emulsion versus the gelatin
solution. Droplet wetting capacity is the key factor for
nucleation of the uidized bed-coating process. As the
wetting capacity improves, so does the coating quality.
Figure 5 shows the effect of gelatin concentration on the
accumulative release of avor over time. When the concentration of gelatin was below 5%, the release value became
close to 100% after 1 min. As the gelatin concentration
increased, the powder sustainably released menthol. For
a gelatin concentration of 15%, it takes 5 min for the
accumulative release of more than 60%, with an initial
release value of 37%. Figure 5 shows the effect of oil
addition on the accumulative release of avor over time.
As oil is added, initial release declines and the time required
for more than 60% release was sustained. When oil content
was 20% based on the weight of gelatin, it took 11 min for
the accumulative release of more than 60% with an initial
release value of 37%.
On the one hand, droplet size increases as viscosity
increases; this effect is caused by the decrease of powder

TABLE 1
The properties of gelatin=gelatin emulsion solutions
Properties
Water
2% gelatin
5% gelatin
10% gelatin
15% gelatin
5% emulsion
10% emulsion
15% emulsion
20% emulsion

Density (g=cm3)

Viscosity (mPa  s)

Surface tension (mN=m)

Powder contact angle (
)

1.001
1.014
1.026
1.057
1.089
1.025
1.02
1.018
1.016

0.467
1.747
3.835
16.82
126.3
1.86
2.497
5.964
10.9

66.155
48.846
42.117
38.502
32.807
48.983
47.102
45.598
43.324

44.432
61.859
58.376
35.74
24.645
58.345
53.234
48.757
43.401

All samples were determined at 60
C.

FLUIDIZED BED-COATED MENTHOL POWDER

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contact angle of the coating solution, which improves the

wettability of the powder surface. On the other hand,
interaction between oil droplets and the hydrophobic
group of gelatin impairs the hydrophilicity of the gelatin
lm, leading to slowed release of avor from the coating
powder. These results indicate that, compared with
AquaCoat ECD, gelatin used as the coating solution
plays a limited part in the controlled release of avor,
though the gelatin coating prolongs the release. Furthermore, addition of oil can enhance the gelatin lm to
better control avor release.
Microencapsulation Efficiency of the Encapsulated
Powder-Coated Gelatin/Gelatin Emulsion
The higher avor content of spray-dried products is
advantageous for the powder products. Therefore, the
effect of the coating solution on microencapsulation
efciency during the uidized bed process was studied
and is shown in Fig. 7. The menthol powder avor with
SSOS by spray drying has almost the same efciency as
the powder produced by Soottitantawat et al.[25] Furthermore, the C1 spray-dried powder has an efciency of
almost 87%, which is less than C2, the powder coated by
the water-coating process. This result indicates that menthol
retention still remains, regardless of losses in the uidized
bed-coating process by the heat, humidity, and agglomeration that inevitably occur during the uidized bed process.
Other than loss of surface volatile avor and agglomeration, the observation of the decline of menthol content
exposed on the powder surface is another factor to explain
growth after the uidized bed-coating process.[26]
Figures 7A and 7B show that microencapsulation efciency
increases with increasing gelatin concentration, while
addition of oil barely inuences efciency. This result might
be explained by the viscosity increase as gelatin concentration increases, which leads to a higher chance of interaction between the droplet and powder, and allows for easier
droplet spreading on the surface of the powder.
CONCLUSIONS
Coating powers prepared by a uidized bed were better
than those prepared by spray drying for controlling the
release of menthol in water. Particles were encased within
gelatin emulsions, which were compared to other coating
materials. These results indicated that the solubility and
integrity of the coating were key factors for the success
of the uidized bed-coating process. Degradation-activated
release from encapsulated powders was achieved by the
uidized bed process. This degradation-activated release
system is applicable in the food industry, because many
foods such as chewing gum and candy are expected to
control the release of their avor during mastication and
swallowing.

1625

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