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2, Mei 2011 (399‐404) ISSN : 1978 ‐ 8193
Abstract
Tofu, a food product made from soybean, contain water and it is very easy to overgrown microbes.
Based on a survey, many products of tofu contain formaldehyde as preservative. Formaldehyde is a
preservative that the use is prohibited for food because it can cause cancer in humans. The aim of this
study was determined concentration of formaldehyde in tofu from traditional market Ciputat using
Spectrophotometer UVI-VIS. Steam distillation was used for sample extraction process. Distillate was
reacted with Nash reagent. The equation of calibration curve is y=0,0032x – 0,0079 and correlation
coefficient of the linear regression of 0,9992. The experimental results obtained LOD value of
11.1328 µg/ml, LOQ value of 37,1094 µg/mL The precision of this analytical method were lower than
2% for each of the sample, while method’s accuration for tofu was 98,69% ± 0,4085%. Results of
sample analysis from Ciputat market, samples were detected containing formaldehyde. Formaldehyde
concentrations are 104,87 µg/mL, 11,21 µg/mL, 1,96 µg/mL, 190,80 µg/mL, 201,98 µg/mL, 10,47
µg/mL, and 3,31 µg/mL.
399
Determ
mination Of Formaldehydee Zilhadia, et.al.
testing of 700 foood products from Jaava, Merck), soluution of 10% phosporic acid
(M
Sulaweesi and Lamppung conduccted in 2002 is Merck), soy bean, Calccium Sulphaate/Sioko,
(M
foundeed that 56 6 % of sample
s contain A
Aquadest.
formaldehyde.
Sample
S
There are 3 laws prohhibit the usee of
T samples are tofu from Ciputat trraditional
The
formaldehyde, firstt UU no 7/11996 about food f
m
market that aree taken randoomly.
and UU U no 8/1999 9 about consuumer protection.
The seecond one, minister
m of heealth regulatiions
Preparation of
P o Tofu simulation
no. 1168/Mennkes/PER/X/11999 staates
S
Soybeans as much
m as 1 kg was washed by
b water,
formaldehyde is a prohibited
p foood additives. The
T
thhen soaked with
w water for
fo approximaately 5-6
thidr one,govermen
o nt regulations about regardding
h
hours. Soybeeans crushedd using a blennder with
food saafety dan nutrritional qualitty no 28 on 2004
added of warm m water (soyya and waterr ratio is
( Depkkes RI BPOM M 2003).
1:2). Soybeans that was cruushed was warmed
w to
Based upo on those regulations,
r we 70-800C in thhe waterbath and filtered. Filtrat
conduccted the ressearch abouut determinattion w warmed again
was a and addded CuSO4 until the
formaldehyde conteent in tofu thhat circulatedd in blob was formed.Tofu
f is ready for the
Ciputaat Market. Tho ose tofu are suuspected conntain compacted.
formaldehyde as preservative.
p We determiined
Ciputaat market becaause it near from
f UIN Syyarif Measure of maximum
M m wavvelength.
Hidayaatullah Camp pus and it is one of the big A solution of 1 ml formaldeehid 150 ppm m inserted
traditioonal market in
n Jakarta so that
t this reseaarch too test tube annd adjusted with
w water unttil 10 ml.
is purrposed as UIN U contribuution to peoople T solution added
The a Nash reagent 5 ml, and then
0
aroundd campus. k
kept at 37 C in waterbbath for 30 menits.
Determinatiion of formaaldehide conntain M
Mixtures movved to volummetric flask 255 ml and
in sam
mple is condu ucted by coloorimetry methhod, adjusted with water until 255 ml, and shaaked until
with Nash
N reagentt which conntain ammoniium h
homogeneus. Maximum wavelengtth was
acetatee, glasial aceetic acid, acetyl aceton and m
measured by UV-Vis
U spectrrophotometerr.
water, as the reagennt. As we knoow formaldehhyde
with acetyl
a aceton
n will condeence to form m a Making Caliibration Cu
M urve and Measured
M
yellow
w 2,6-dimetil-3,5-diasetil-1,4-dihidropiriidin L
Linieritas.
compoound. This compoundd has grreen M
Making calibrration curve is done by methods
floureccence color thhat can be deetected in visible thhat was saame as measure of maximum m
wave ata 412 nm. w
wavelength. Absorban of soluttion of
foormaldehid ono a series of
o concentratiion was
m
measured at thhe maximum wavelength.
2. M
METHODOL
LOGY Limit of Deetection (LO
L OD) and Limit
L of
Instruments Q
Quantitation (LOQ)
Squashh, distilation equipment, gas distilattion T limit of detectin
The d wass calculated using
u the
equipmment, measuring cupps, erlanmeyyer, foormula
thermoometer, test tube,watchh glass, metal m
spatulaa, analyticcal balancee, alumuniium LOD =
foil,disssposable glloves, maskks, petri dish,
d
volumeetric pipettte, waterbbath, UV--Vis
The Limit of Quantification
T Q n was calculaated using
spectroophotometer.
thhe formula:
Material
Formallin (Merck) 37% (waater solution of L
LOQ =
formaldehyde), Ammmonium acetate
a (Merck),
Acetic acid glaciaal (Merck), acetyl acettone S
Sy/x is standarrt deviasion
400
Valensi Vol. 2 No. 2, Mei 2011 (399‐404) ISSN : 1978 ‐ 8193
Analysis of Samples
For the analysis of samples out of the market
Ciputat used the same method to measure out the
simulation.
412.73
or release the bond between formaldehyde with
proteins so the formaldehyde can be separated by
0.8
0.7
0.6
0.4
0.3
0.1
0.00
300.0 320 340 360 380 400
nm
420 440 460 480 500.0 submerged into the water cooler end. It aims to
capture the formaldehyde vapor generated into
Figure 1. The maximum wavelength of solution the water distillation process that has been
of formaldehid which reacted with Nash Reagent
401
Determination Of Formaldehyde Zilhadia, et.al.
Absorbansi
0.6 Linear…
analytical method begins by making the 0.4
calibration curve and determination of linearity. y = 0,0032x - 0,0079
0.2
Calibration curve is the relationship between the R² = 0,9992
absorbance value of the analyte to the 0
concentration of the analyte. The linearity is the -0.2 0 200 400
Konsentrasi (ppm)
ability of analytical procedure to produce test
results which are proportional to the
concentration (amount) of analyte in samples Figure 2. Formaldehyde calibration curve in a
within a given concentration range, either series of concentration (ppm) against absorbance
directly or by means of a well-defined
mathematical transformation. The value of
correlation coefficient (r) is good if it is 0.999. Accuracy is the closeness of the results
This means increasing the value of the analyte obtained by determination of actual results and
absorbance is directly proportional and expressed in percent recovery. Percent recovery
significantly with increasing concentration. of three different concentrations of formaldehyde
calibration curve generated with the equation Y are 99.14% for the concentration of 125 µg/ml,
= 0.0032 x - 0.0079 and correlation coefficient 98.59% for the concentration to 175 µg/ml and
(r) = 0.9992. Formaldehyde calibration curve in 98.36 % for the concentration of 225 µg/ml. The
a series of concentration (ppm) against average of percent recovery is 98.69% with
absorbance can be seen in Figure 2. standard deviation (SD) of 0.4086. Recovery test
requirement is 98-102%, so the results of this
Limit of Detection (LOD) is the lowest test meets the requirements. Results of Recovery
analyte concentration in the samples can still be test of formaldehyde in tofu simulation can be
detected (Gholib, 2006). The experimental seen in table 2.
results obtained LOD value of 11.1328 µg / ml.
Limit of quantitation (LOQ) is the smallest Table 2. Results of Recovery test of
quantity of analyte in the samples can still be formaldehyde in tofu simulation.
determined by the method used and meet the
criteria carefully and thoroughly. The LOQ Concentration Percent of Average
values obtained of 37.1094 g / ml. The result of (µg/ml) Recovery ±SD (%)
the calculation of LOD and LOQ can be seen in 125 99,14
table 1. 98,69 ±
175 98,59
0,4085
225 98,36
Table 1. The result of the calculation of LOD
and LOQ
Results of precision test of formaldehyde in the
∑ (y - y)² 0,00042294 tofu simulation can be seen in table 3.
S(y/x)² 0,00014098
S(y/x) 0,011875
LOD (Limit Of Detection) 11,1328 µg/ml
LOQ (Limit Of Quantitation) 37,1094 µg/ml
402
Valensi Vol. 2 No. 2, Mei 2011 (399‐404) ISSN : 1978 ‐ 8193
X = 98,69 ∑ 0,3339
ACKNOWLEDGMENT
This research supported by Departement of
The standard deviation (SD) of data obtained at Pharmacy, Faculty of Medicine and Health
0.4086 and coefficient of variation (CV) of Science, UIN Syarif Hidayatullah Jakarta.
0.4139%. Coefficient of variation requirement is
<2%, so the results of this test meets the
REFERENCES
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method could be used for samples analysis
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Determination Of Formaldehyde Zilhadia, et.al.
404