Electronic Sensing of Aromatic Volatiles for
Quality Sorting of Blueberries
JAMES E. SIMON, AMOTS HETZRONI, BRUCE BORDELON, GAINES E. MILES, and DENYS J. CHARLES
ABSTRACT
An electronic sniffer using semi-conductor gas sensors that nondestruc-
tively measured aromatic volatile gas emissions from fruit was devel-
oped to assess blueberry quality. The sniffer detected soft and damaged
fruit in packaged containers at a 5% level of damage and distinguished
four of five fruit ripeness classes: (1) mature-green and green-pink; (2)
blue-pink; (3) blue; and (4) ripe fruit. Sniffer response increased as fruit
ripened, as did total concentration of aromatic volatiles. Sniffer response
correlated with berry firmness, pH, titratable acidity, and color, and de-
tected differences among 10 cultivars, as did impact response analysis.
The electronic sniffer is rapid, nondestructive and may be used to sort
and quality check for presence of unripe or damaged fruit in closed packs
of fresh berries.
Key Words: blueberries, conductivity, volatiles, aroma, odor sensing
INTRODUCTION
NONDESTRUCTIVE TECHNIQUES to determine blueberry quality in
a consistent and reproducible manner would benefit the blueberry
industry and consumer. As a highly perishable fruit, blueberries
must be harvested at the proper time, sorted and graded, pack-
aged, cooled, shipped and properly stored until sold and processed
or used by the consumer (Gough, 1994). Quality control is nec-
essary with all fresh produce, but is of particular importance to
small fruits. Traditional systems of human classification (visual
assessment of color, size, uniformity and defects such as cracks,
leaks, and soft berries) are effective but time-consuming and dif-
ficult to quantify or verify. Highly perishable fruit, once graded
and packaged, may develop damage (e.g. cracks, leaks, softs,
spoilage) that would be noticed only by the end-user. An elec-
tronic sensory system, which indirectly measured the total aro-
matic volatiles of fruit has been developed that permits nonde-
structive sampling of volatiles in a rapid and reproducible manner.
The electronic sniffer was originally developed at Purdue Uni-
versity to predict ripeness of muskmelons (Benady et al., 1995),
and has also been effective with a wide range of other fruit in-
cluding apples and strawberries (Benady et al., 1995; Hetzroni
et al., 1994, 1995).
The electronic sniffer is based on a semi-conductor designed
to react with a range of reductive gases, such as aromatic vol-
atiles naturally emitted when fruit ripen (Benady et al., 1995).
The surface of the semi-conductor is coated with tin dioxide (n-
type) that has a low conductivity in clean air. In the presence
of reducing gases, oxygen is displaced from the surface and re-
placed with the other gases, increasing the conductivity. The
change in conductivity measures the concentration of total vola-
tiles. The electrical resistance of semiconductor gas sensors de-
creases with increasing gas or vapor concentration in the ambient
atmosphere. As conductivity increases so does the sniffer re-
sponse (mV), while the sniffer response when expressed as Rs/
Ro decreases. A detailed description and illustration of the system
with melons has been reported which demonstrated the relation-
ship between the electronic sniffer response and volatile emissions
Authors Simon, Hetzroni, Bordelon, and Charles are with the Cen-
ter for New Crops and Plant Products and author Miles is with
the Dept. of Agricultural and Biological Engineering, Purdue
Univ., West Lafayette, IN 47907.
Volume 61, No. 5, 1996—JOURNAL OF FOOD SCIENCE—967
(Benady et al., 1995). Other research groups using semi-con-
ducting technology and other gas sensors have assessed quality
in aroma and flavor of beverages and changes in processed
foods. Electronic sensing of volatiles has detected alcohols and
tobacco smoke (Shurmer et al., 1989), coffee (Gardner et al.,
1990), perfumes and flavors (Nakamoto et al., 1993), fish
(Olafsson et al., 1992), beer (Tyler et al., 1994), and fruit ripe-
ness (Benady et al., 1994; 1995; Hetzroni et al., 1994, 1995).
Coupled with statistical pattern recognition techniques, this odor
sensing technology has wide applications in fresh produce and
food quality assessment.
More than 50 volatile compounds are associated with blueber-
ries, but only 5 have been shown to be associated with the aroma
and flavor of fresh berries. Parliment and Kolor (1975) found that
(E)-hex-2-enal, (E)-hex-2-enol and linalool were associated with
the sensory characteristic flavor of fresh blueberries. Later, Horvat
and Senter (1985) extracted 51 volatile compounds from blue-
berries, and among them, (Z)-hex-3-en-1-ol and geraniol also had
typical fruity aromas characteristic of fresh blueberries. These
volatiles increase with fruit maturity (Horvat and Senter, 1985).
These studies did not directly measure volatile gases emitted by
intact blueberries, rather they were based upon destructive ex-
traction techniques. Packs of damaged fruit may also differ in
composition and intensity of volatiles. Compositional changes
in volatiles also occur during fruit ripening and may vary de-
pending on the presence of diseases, physical damage, as well
as extraction/recovery techniques (Hirvi, 1983). Such changes,
if quantified, may be useful as markers in quality sorting (Horvat
and Senter, 1985).
Measurement of volatiles as a quality parameter has been ne-
glected due to the time, high cost and technical difficulties in
the collection and analysis of gas samples. If gas sensors were
sensitive enough to the ambient levels of gas emissions from
fruit, and if the objective were total emission load rather than
quantification of individual compounds, then this semi-conduct-
ing technology could be useful to monitor fruit quality.
Preliminary studies on blueberries suggested that the elec-
tronic sniffer may be used to predict ripeness and quality of
packaged blueberries (Benady et al., 1994). The objectives of
our study were to: (1) determine if the electronic sniffer could
be used in quality sorting of blueberries; (2) determine varia-
bility in sniffer response among cultivars; and (3) determine if
the electronic sniffer could assess blueberry ripeness.
MATERIALS & METHODS
Fruit quality measurements
Fruit quality was measured by nondestructive and destructive meth-
ods. Nondestructive methods included electronic gas sensing, color, and
firmness. Destructive measurements included firmness, total soluble sol-
ids, pH and titratable acidity. Each cultivar was replicated six times using
'551 cc clam shell packs (ca. 355g of berries) containing 130-350 ber-
ries/pack (cultivar dependent), unless otherwise noted.
The electronic sniffer
Our unit consisted of a rectangular chamber (4017 cc) with a remov-
able lid into which the sensors were mounted. The chamber could con-
tain a single '551 cc ‘clam shell’ plastic container, the typical size and
type used commercially for blueberries. Two tin oxide (n-type) gas sen-
QUALITY SORTING BLUEBERRIES BY AROMATIC VOLATILES . . .

Table 1—Physicochemical properties associated with blueberry ripening

Total
HeadSpace soluble Juice Sniffer
Ripeness Firmness Hue L a b volatilesz solidsy pH TAx responsew
Mature-green 28.7 av 109 b 56.8 a 210.9 d 26.9 a 6.25 b 6.8 d 2.88 d 2.15 c 4.60 a
Green-pink 17.2 b 79 c 50.7 b 5.2 b 15.3 b 6.60 b 7.8 c 2.91 d 2.22 c 4.76 a
Blue-pink 4.5 cd 284 a 34.7 c 9.3 a 22.4 c 11.32 a 8.9 b 3.00 c 1.44 b 4.21 b
Blue 4.2 d 288 a 34.2 c 1.6 bc 24.3 c 11.18 a 9.3 b 3.16 b 1.00 a 3.93 c
Ripe 7.7 c 274 a 33.6 c 0.2 c 25.1 c 12.45 a 10.2 a 3.26 a 0.86 a 3.70 d
z Total GC peak area (X1,000).
y TSS values arc sin transformed for statistical analysis, actual percentage means provided.
x TA 5 titratable acidity.
w Sniffer 5 Rs/Ro
v Mean values in same column followed by same letters not significantly differnt by Duncan’s Multiple Range Test (P,0.05).

Table 2—Pearson correlation of measured properties of blueberries, cv Chemical characterization of aromatic volatiles
Bluecropz
SS pH TA Firmness L a b Hue Direct injection of headspace gases. To capture headspace gases,
Sniffer 20.68 20.85 0.88 0.62 0.70 ns 0.71 20.73
blueberries (40g) were placed into a 120 cc jar for 18 hr, then a 4 mL
SS 0.78 20.76 20.76 20.74 0.39 20.81 0.71 gas sample was removed with a syringe and injected into the GC.
pH 20.92 20.66 20.76 ns 20.79 0.72 Volatile compound identification and quantification by GC. The
TA 0.76 0.85 ns 0.86 20.85 dichloromethane extracts were analyzed by using a Varian 3700 GC
Firmness 0.92 20.71 0.95 20.81 equipped with FID and a Varian 4270 integrator. Compound verification
L 20.62 0.98 20.87 was achieved using GC/MS, connected on-line with a Data General
a 20.64 ns Nova/4 data processing system, implementing electron impact analysis
b 20.86 (Charles et al., 1990; Charles and Simon, 1990). Identification of volatile
z All values significant at p,.01 2 p,.0001; ns 5 not significant, thus, no correlation
constituents was accomplished by matching the mass spectra of each
value reported. compound with spectra from MS compound libraries for best fit (Charles
et al., 1991).
Studies on ripeness determination. Locally produced blueberry fruit
sors (TGS 822; Figaro Eng. Inc., Osaka, Japan) were used to provide an cv. Bluecrop, were hand harvested at a commercial farm (Lafayette, IN)
average reading. The electronic sniffer required a conditioning circuit and manually sorted into five ripeness classes: mature-green, green-pink,
and the sensor output was acquired by a data acquisition board attached blue-pink, blue, and ripe (Eck et al., 1990). Berries were evaluated using
to a portable computer. Packed blueberries (551 cc) were placed into the the electronic sniffer, the color-meter, compression test, TSS, pH, and
chamber which was then sealed. A fan inside the chamber circulated air. TA. Each ripeness class was replicated eight times, and each sample
Headspace gases emitted from the fruit were continuously measured by contained 100g berries.
the sensors over a preselected time. The chamber and sensing head were Variability in sniffer response and IRA among blueberry culti-
flushed with compressed nitrogen between samples. Samples were meas- vars. Ten blueberry cultivars (Berkeley, Bluecrop, Blueray, Coville,
ured continuously for 64 sec, immediately after the lid was sealed onto Darrow, Elliott, G-344 (USDA), Jersey, Nelson, and Rubel) were har-
the chamber. Voltage output from the sensors was recorded at 0.5 Hz. vested manually, sorted and graded into US No. 1 fruit by expert graders
Typical response from the gas sensors when exposed to the volatile at MBG Marketing (Grand Junction, MI). Fruit were then placed into
reducing gases of fruit can be described in an exponential function model '551 cc containers (ca 355g berries) and the fresh weight recorded.
in which the sensor response (voltage output, mV) increases during a Berry packs were evaluated with the electronic sniffer and IRA. Each
transitional period and then stabilizes. Empty plastic containers were also cultivar was replicated six times.
originally sampled and did not induce signal response by the sniffer. All Detection of damaged fruit. To determine if damaged berries (soft
calculations in this paper were performed with normalized sensor re- or leaky fruit) could be detected in a closed package, fruit (cv. Bluecrop)
sponse values as Rs/Ro, where Rs is the sensor resistance at different were first manually sorted and only high quality ripe fruit (exceeding
concentrations, and Ro is the sensor resistance at 300 ppm ethanol, used US No. 1 grade) were gently placed into the containers and evaluated
as the reference standard for each gas sensor. by electronic sniffer. After gas sensing (electronic sniffer), in each con-
tainer we replaced good berries with damaged berries (leaky and soft),
and then reevaluated them by the electronic sniffer. The replacement
Fruit color levels evaluated were 0, 5, 10 and 20% damaged fruit by weight.

Color was measured on 10 randomly selected berries from each pack.

All color measurements were recorded in the L, a, b space, using a
Minolta CR-200 colorimeter with C illuminant. Hue was calculated from
these values.
Fruit firmness
A ‘BerryBounce’ unit (McGlone and Schaare, 1993; Patel et al.,
1993), was used to assess fruit firmness (nondestructive) of all berries
in each pack. This unit measures contact time of berries bouncing off
an impact plate and is termed ‘Impact Response Analysis’ (IRA). A
destructive firmness assessment by a compression test used single berries
held onto a firm surface, while an 11 mm plunger attached to Chatillon
strain gauge was slowly lowered through the berry. The peak compres-
sion force (or penetrating force) required to cause berry rupture was
measured.
Fruit composition
Total soluble solids (TSS) of the juice were measured by a tempera-
ture compensated refractometer. Juice was expressed from 100g berry
samples with a ‘Squeezo’ fruit juicer. The pH of juice was measured by
a Corning pH Meter 220. Titratable acidity (TA) of the juice was deter-
mined by titration to pH 8.2 with 0.1N NaOH.
RESULTS & DISCUSSION
AS BLUEBERRY FRUIT RIPEN, firmness decreases, and the hue
increases as illustrated with cv. Bluecrop (Table 1). The ‘b’
color measure (blue to yellow) was most indicative of blueberry
color. Separation into three ripeness stages based upon color was
consistently achieved as shown with the ‘L’ and ‘b’ scales (Ta-
ble 1). This was expected, as fruit were separated primarily
based upon visual color by a human grader. Compression as a
measure of firmness differentiated four distinct ripeness classes,
and was most efficient in separating the less mature fruit (mature
green vs green-pink vs blue-pink). The electronic sniffer was
also successful in separating blueberries based upon ripeness.
The electronic sniffer separated the fruit into four ripeness clas-
ses as were based upon color: (1) mature-green and green-pink;
(2) blue-pink; (3) blue fruit; and (4) ripe fruit (Table 1), indicating
the potential for the sniffer to distinguish between ripe and unripe
fruit. Although it did not separate mature-green and green-pink
classes, the sniffer separated the classes of mature berries (blue-
pink vs blue vs ripe). Sniffer response (mV) increased with fruit
ripening, as did the total concentration of aromatic volatiles, sup-
porting the hypothesis that aromatic volatiles increase with fruit

968—JOURNAL OF FOOD SCIENCE—Volume 61, No. 5, 1996

 Table 3—Cross validation summary using linear discriminant function for classifying blueberries into five ripeness classes using destructive and
nondestructive measurements (firmness, hue, L, a, b, TSS, pH, TA and the electronic sniffer) as classification parameters
3A. 3B.
To ripeness To ripeness
From ---------- (all factors)z ---------- From ---------- (without SS)y ----------
ripeness MG GP BP B R ripeness MG GP BP B R
Mature-green (MG) 7 1 0 0 0 Mature-green (MG) 8 0 0 0 0
Green-pink (GP) 3 5 0 0 0 Green-pink (GP) 1 7 0 0 0
Blue-pink (BP) 0 0 4 2 2 Blue-pink (BP) 0 0 8 0 0
Blue (B) 0 0 1 5 2 Blue (B) 0 0 0 7 1
Ripe (R) 0 0 1 1 6 Ripe (R) 0 0 0 0 8
z Percent classification error 5 32% for all nine factors.
y Percent classification error for eight factors, all except for total soluble solids 5 5%.

Table 4—Electronic sniffer response from packed and graded blueberries Our major objective was to determine whether the electronic
(cv. Bluecrop) with soft and leaking fruit added
sniffer could be used in the quality sorting of packaged blue-
Added level No. Sniffer berry fruit. As such, the sniffers’ capability to detect soft fruit
(% by wt) samples responsez
and leakers present within a packed container of blueberries was
0 11 7.79 ay
5 12 5.86 b
evaluated. A significant increase in sniffer response was
10 12 5.13 c achieved at a 5% addition of defective fruit (Table 4). As the
20 12 5.10 c defect level (10% and 20%, respectively) increased, so did the
z Sniffer 5 Rs/Ro respective sniffer response. These data show that the sniffer had
y Mean separation by Duncans Multiple Range Test at P 5 0.05.
the potential for detecting damaged fruit at least at the 5% defect
level in commercial packs. The lowest detectable threshold level
of damaged fruit was not determined.
Table 5—Response of different cultivars to electronic sniffer and impact
response analysis Blueray, Berkeley, Coville, Bluecrop, Darrow and G-344 ex-
Sniffer response
hibited the highest sniffer response; Nelson, Jersey and Rubel
Cultivar Rs/Ro Impact response analysisz the least (Table 5). These results indicated that the sniffer could
Berkeley 5.86 cy 1.57 c operate across a wide range of blueberry cultivars, but that base-
Bluecrop 6.46 bc 1.69 bc line data for each cultivar could be required to compensate for
Blueray 5.77 c 1.63 bc differences and achieve accurate prediction or interpretation of
Coville 5.87 c 1.27 d responses. Cultivar differences were also noted based on IRA
Darrow 6.67 bc 2.39 a
Elliottx 8.12 1.60 from the BerryBouncer, suggesting that other nondestructive
G-344 (USDA) 6.92 b 1.75 b methods were also cultivar dependent.
Jersey 8.44 a 1.79 b Volatiles from the ripe fruit of nine cultivars were also obtained
Nelson 8.58 a 2.35 a via dichloromethane extraction and analyzed by GC and GC/Mass
Rubel 7.88 a 1.12 d
z milliseconds
Spec. Extraction by solvents, as performed on each cultivar at a
y Mean values in the same column followed by same letters are not significantly dif- single stage of ripeness (ripe), yielded 12 main volatile constitu-
ferent by Duncan’s Multiple Range Test (P,0.05). ents which we report here tentatively as: E-hept-3-enal; 2,3,5-
x Elliott was harvested at a different time period, thus, not included in the overall sta- trimethylheptane; 1,8-cineole; 2,4-dimethyl-5-ethyl-hept-2-ene;
tistical analysis. nonanal; camphor; menthone; 2,6-dimethoxyphenol; decanoic
acid; a-cubebene; valencene; and hexadec-4-en-6-yne. Only two
of these compounds, 1,8-cineole and nonanal, were previously
maturation. These results were consistent with our observations reported (Horvat and Senter, 1985; Hirvi and Honkanen, 1983).
on apples, melons and strawberries (Benady et al., 1995; He- Differences in extractable volatiles between our study and others
tzroni et al., 1994, 1995). Blueberries emit a low level of aro- may in part relate to extraction techniques as well as cultivars.
matic volatiles relative to other fruits, and our headspace gas Parliment and Kolor (1975) used vacuum steam distillation, fol-
system captured only two aromatic volatiles (butyl acetate and lowed by extraction with ether and concentration by distillation;
2-butoxyethanol) in addition to CO2 from the ripe fruit (Table Horvat and Senter (1985) employed a continuous Likens-
1). While butylacetate is a common aromatic volatile of fruit, Nickerson steam distillation followed by pentane extraction;
2-butoxyethanol has not been previously reported. Since it is a Hirvi and Honkanen (1983) used thawed berries which were
common solvent, we suspect it was an artifact in either the am- pressed and extracted using redistilled diethyl ether-pentane.
bient air or on the blueberry fruit. As blueberry fruit ripen, there
was a concurrent increase in aromatic volatiles (Table 1).
Nine measurements of fruit quality and ripeness were subjected
to Pearson correlation analysis (Table 2), and the gas sensor was CONCLUSIONS
significantly correlated with color (L, b, and hue), firmness, TA, THE ELECTRONIC SNIFFER provided a rapid, nondestructive ap-
pH, and TSS. A cross-validation discrimination analysis (SAS proach to sort blueberry fruit for quality. It detected immature
Institute, Inc., 1995) for classifying blueberries into five ripeness from mature fruit, separated mature fruit based on ripeness, and
classes using both destructive and nondestructive measurements detected damaged fruit in a closed container of fresh berries.
indicated a 32% error in ripeness classification when all factors The electronic sniffer may have application for both quality con-
were included (Table 3A). Stepwise discrimination analysis was trol and prediction of shelf life and be useful in the grading and
conducted, and determined that soluble solids could be elimi- sorting of fresh fruit.
nated, thus reducing classification error from 68% to 5% (Table
3B). The focus of our work was to use nondestructive measure-
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This study was funded by the Michigan Blueberry Growers Marketing (MBG); the Com-
mission of Agriculture, State of Indiana; the Center for New Crops and Plant Products, Purdue
University, and a grant from BARD (No. US-2234-92R).
We thank Dave Trinka, who facilitated our research at MBG and who made arrangements
for the collection of blueberry fruit >ny Benady who was central in the preliminary studies
the preceding year of this project; Gary Gao, who assisted in some of the initial volatile
extraction studies d̊ Marshall Martin for blueberries.