spectrophotometric determination of nicotine in
TRANSCRIPT
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Omara et al. World Journal of Pharmacy and Pharmaceutical Sciences
SPECTROPHOTOMETRIC DETERMINATION OF NICOTINE IN
CIGARETTE TOBACCO AND BIOLOGICAL SAMPLES OF
SMOKERS
Hany A. Omara* and Salma M. M. Attaf
Chemistry Department, Faculty of Science, Sirte University, Sirte, Libya.
ABSTRACT
A new simple, accurate, sensitive and economical procedure for the
estimation of nicotine (indirect) methods (A and B) for the
determination of nicotine in bulk sample and in biological samples are
described. The first method is based on the oxidation of nicotine by N-
bromosuccinimide (NBS) and determination of the unreacted NBS by
measurement of the decrease in absorbance of methyl orange dye
(MO) at a suitable λmax = 507 nm. The absorbance concentration plot is
linear over the range (0.1-4.8 µg/ml). The second method is based on
oxidation of nicotine by cerric sulphate in acidic medium, and
determination of the unreacted oxidant by measuring the decrease in absorbance using
amaranth dye; (AM) at a suitable λmax (530 nm), respectively. Regression analysis of Beer's
law plots showed good correlation in the concentration ranges (0.3-5.9 µg/ml), respectively.
The limits of detection as well as quantification are reported. Sex replicate analyses (n=6) of
solutions containing three different concentrations of nicotine was carried out. The percent
error and the RSD values have been reported. The proposed methods were applied to the
determination of nicotine in cigarette tobacco present in Libya and in biological samples
(spiked human plasma and urine) and the results demonstrate that the method is equally
accurate and precise as found from the t- and F-values. The reliability of the method was
established by recovery studies using standard-addition technique.
Key Words: Nicotine; Spectrophotometry; Oxidation reaction; N-bromosuccinimide; Cerric
sulphate, Cigarette tobacco in Libyan markets; Spiked human plasma and Urine.
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Article Received on 17 May 2014, Revised on 12 June 2014, Accepted on 23 July 2014
*Correspondence for Author
Dr. Hany A. Omara
Chemistry Department, Faculty
of Science, Sirte University,
Sirte, Libya
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INTRODUCTION
Nicotine (pyridine, 3-(1-methyl-2-pyrrolidinyl), (S) is one of the highly toxic tobacco
alkaloids present in tobacco leaves and cigarette smoke [1]. Nicotine appears to be a
promising tracer for environmental tobacco smoke (ETS) because of its specificity for
tobacco [2]. It is also a systemic and contact insecticide and is also used as a drug and in
chemical [3]. The threshold limit value reported for nicotine is 0.05 mg/m3 [1]. The most
important symptoms of exposure to nicotine are bronchitis, emphysema, cyanosis, and
exenation of the central nervous system. Excessive smoking has been implicated in lung
cancer, bladder cancer, and cancer of the larynx and oesophagus [4].
The determination of total nicotine alkaloids is of particular importance to the tobacco
industry and in the area of toxicology. Various analytical methods such as GC [5], TLC [6],
HPLC [7-9], ASS [10], capillary electrophoresis [11], radio immuno assay [12], GC-MS [13] and
circular dichroism spectropolarimetry [14] have been reported. Most spectrophotometric
methods reported are based on cleavage of the pyridine ring with cyanogen bromide or
chloride and condensation of the resulting compound with p-amino benzoic acid [15] and
diethyl thiobarbituric acid [16] and other spectrophotometric methods [17-24], determination of
outdoor Tobacco smoke exposure by distance From a smoking source [25 ], an
electrochemically [26].
Many of these methods involve a prolonged extraction procedure prior to the determination
of nicotine and the use of highly toxic cyanide [15, 16]. These methods were sophisticated to
perform and/or time consuming. The oxidation reaction between NBS or Cerric in acidic
medium and nicotine have not been investigated yet but for other drugs [27-37].
EXPERIMENTAL
Apparatus
All the spectral measurement were made using double-beam UV/Vis spectrophotometer
(Biotech Engineering Ltd., UK), with wavelength range 190 –1100 nm, spectral bandwidth
2.0 nm, with scanning speed 400 nm/min, equipped with 10 mm matched quartz cells. A
thermostat water bath, Buchi 461 water bath, Schwiz (France) was used to carry out the
temperature studies and Magnetic Mix. 100, Thermo Scientific, UK.
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Material and reagents
All chemicals used were of analytical reagent grade of the best available quality. and all
solutions were freshly prepared in doubly distilled water.
Standard nicotine solution (Merck) was prepared by dissolving 0.01 g of pure nicotine in 50
ml of bi-distilled water and complete to 100 ml with bi-distilled water to obtain the working
standard solution of 100 µg/ml.
A stock solution of 1.0 x 10-3 M NBS (Aldrich Co., Ltd., Gillingham-Dorst, Germany) was
freshly prepared by dissolving 0.0177 g of NBS in a least amount of warm water in a 100 ml
measuring flask and then diluted with distilled water to the mark.
A stock solution of 1.0 x 10-3 M cerric sulphate (Aldrich Co., Ltd., Gillingham-Dorst,
Germany) was freshly prepared by dissolving appropriate weight of Ce (VI) in a least amount
of warm water in a 100 ml measuring flask and then diluted with distilled water to the mark.
A 2.0 M of HCl was prepared by adding exact volume from stock concentrated acid to
bidistilled water in 500 ml measuring flask (Merck, Darmstadt, Germany, sp. gr. 1.18%,
37%) to 100 ml with distilled water.
A solution of 2.0 M H2SO4, was prepared by adding exact volume from stock (98%)
concentrated acid to bidistilled water in 500 ml measuring flask, and standardized as recorded [38].
Aqueous solutions of dyes (1.0 x 10-3 M) methyl orange (MO) (Merck), (1.0 x 10-3 M)
amaranth (AM) (Merck) were prepared by dissolving in an appropriate weight in 100 ml
bidistilled water.
General procedure
For the first method, (method A) depends on oxidation of nicotine by addition of 0.01-4. 8 ml
(100 µg/ml) to 1.8 ml of 1.0 x 10-3 M NBS containing 1.1 ml HCl, 2.0 M. The solution was
heated in a water bath at 80±1 oC for 4.0 min. The solution was cooled and 1.7 ml (1.0 x 10-3
M) of MO was added, the volume was completed to 10 ml with bidistilled water. For the
second method (method B) depends on oxidation of nicotine by addition of 0.01-5.9 ml
nicotine (100 µg/ml) to 1.5 ml of 1.0 x 10-3 M Ce (VI) containing 1.2 ml of 2.0 M H2SO4 was
added. The solution was heated in a water bath at 80±1 oC for 5.0 min, the mixture of acidic
solution was cooled and 1.6 ml (1.0 x 10-3 M) of AM was added, the volume was completed
to 10 ml with bidistilled water. The decrease in color intensity of dye was measured
spectrophotometrically against a blank solution containing the same constituent except drug
treated similarly, at their corresponding λmax 507 (method A), 530 nm (method B),
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respectively. The concentration range was determined in each case by plotting the
concentration of nicotine against absorbance at the corresponding maximum wavelengths.
Extraction and determination of nicotine in cigarette tobacco [39]
Weigh 10 g of cigarettes leaves in beaker. Add 100 ml NaOH solution and stir very well for
15 min, filter in Buchner using glass wool and press the cigarettes very well by using other
beaker, transfer the cigarettes again to beaker, add 30 ml DW and stir and filter again, collect
the filtrate together, (if there is any impurities re-filter), transfer the filtrate to the SF and
extract by 25 ml ether, repeat the extraction 3 times, gather the 4 filtrates in conical flask, dry
by using 1.0 teaspoon anhydrous potassium carbonate, filter. evaporate ether on water bath,
(avoid extra heat because nicotine is hydrolyzed by extreme heating), after evaporation of
ether add 4.0 ml methanol to dissolve the resulted oil, to the filtrate 14 ml of 1.0 mol/L HCl
was added and the solution was made up to 100 ml with water. An aliquot of this solution
was taken and analyzed as described above. The results are shown in Table 2.
Procedure for spiked human urine
A 50 ml volume of nicotine – free human urine taken in a 125 ml separating funnel was
spiked with 2.5 mg nicotine. Ten milliliters of 1.0 M NaOH was added, mixed and kept aside
for 3.0 min. Then, 25 ml of ethyl acetate was added, shaken well for about 15 min and the
upper organic layer was collected in a beaker containing anhydrous sodium sulphate. The
water-free organic layer was transferred into a dry beaker and solvent removed by
evaporation on a hot water bath. The dry residue was dissolved in glacial acetic acid and
transferred into a 25 ml calibrated flask, and diluted to the mark with the same acid. The
resulting solution equivalent to 100 µg/ml nicotine was diluted with the same acid and
analyzed by following the procedure described above.
Procedure for spiked human plasma samples
Aliquots of 1.0 ml of plasma were spiked with different concentration levels of nicotine. The
spiked plasma samples were treated with 0.1 ml of 70% perchloric acid and vortexes for 1.0
min. The samples were centrifuged for 20 min at 13000 rpm. The supernatants were
transferred into test tubes and neutralized with 1.0 M NaOH solution.
Stoichiometric relationship
The stoichiometry of the reaction between nicotine and the oxidants at the selected conditions
were established by the molar ratio method. In this method 1.0 ml of 1.0 x 10-3 M NBS
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(method A) 1.0 x 10-3 M Ce (VI) (method B) is kept constant and variable concentrations
(0.1-6.0 ml) of nicotine (1.0 x 10-3 M) were added. The absorbance was measured at λmax
against blank solution prepared in the same manner. The absorbance values were then plotted
against the molar ratio [D]/[O] as shown in Figure 6.
RESULTS AND DISCUSSION
First Method (A)
The proposed spectrophotometric methods are based on the reaction between nicotine and
measured excess of NBS and subsequent determination of the latter by reacting it with a fixed
amount of MO dye, and measuring the absorbance at 507 nm. The reaction takes place
completely after 4.0 min., was heated in a thermostat water bath at 80±1 oC. This method
make use of the bleaching action of NBS on the dye, the decolorization being caused by the
oxidative destruction of the dye. nicotine when added in increasing concentrations to a fixed
concentration of NBS consumes the latter and there will be a concomitant decrease in the
concentration of NBS. When a fixed concentration of dye is added to decreasing
concentrations of NBS, a concomitant increase in the concentration of dye is obtained.
Consequently, a proportional increase in the absorbance at the respective λmax is observed
with increasing concentrations of nicotine, the color remains constant for at least 48 h.
Second Method (B)
The method involves two steps namely:
Oxidation of nicotine with Ce(SO4)2 in acidic medium by heating in water bath 80±1 oC.
Determination of unreacted oxidant by measuring the decrease in absorbance of dye at a
suitable λmax.
Nicotine + Ce(SO4)2 42. SOHDil Oxidized products + Ce (III) + Ce(SO4)2
(Unreacted)
Unreacted Ce(SO4)2 + Amaranth dye → Ce (III) + Unreacted Amaranth dye
Pink colour, λmax 530 nm
The influence of each of the following variables on the reaction was tested.
Effect of NBS concentration
The influence of NBS concentration was studied in the range from 10-4 - 10-2 M, as final
concentration. The optimum results were obtained with 1.8 ml of 1.0 x 10-3 M.
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0.0
0.2
0.4
0.6
0.8
0.0 0.5 1.0 1.5 2.0 2.5 3.0
ml added of NBS
Abs
orba
nce
MO
0.0
0.2
0.4
0.6
0.8
1.0
0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5
ml added of Ce(VI)
Abs
orba
nce
AM
Effect of cerric sulphate concentration
The influence of Ce (VI) concentration was studied in the range from 10-4 - 10-2 M, as final
concentration. The optimum results were obtained with 1.5 ml of 1.0 x 10-3 M; higher
concentration of Ce(SO4)2 caused the color to disturbed.
Effect of acid medium
The different types of acid were examined (HCl, HClO4, H2SO4, H3PO4, CH3COOH and
HNO3). The most suitable acid to achieve maximum yield of redox reaction was found to be
1.1 ml of 2.0 M HCl for (method A) and 1.2 of 2.0 M H2SO4 was added on using AM, for
(method B) Figure 3.
Fig. 1. Effect of ml added of NBS (1 x 10-3 M);
nicotine (4.0 µg/ml) 1.1 ml of 2.0 M
hydrochloric acid, reaction temperature
80±1 °C; reaction time: 4.0 min
Fig. 2. Effect of ml added of Ce (VI) (1 x 10-3 M)
(10 M) on 4.0 µg/ml nicotine, 1.2 ml of 2.0 M
sulphoric acid; reaction temperature 80±1 oC;
reaction time: 5.0 min
Effect of temperature and time
The reaction takes place completely after 20 min at room temperature 25±1 oC. The oxidation
process of nicotine with NBS is catalyzed by heating in a thermostat water bath at 80±1 oC
for 4.0 min. using MO dye. The oxidation process of nicotine for the (method B) Ce(SO4)2 in
acidic medium was catalyzed by heating in a thermostat water bath of 80±1 oC for 5.0 min,
using AM. After oxidation process, the solution must be cooled at least for 2.0 min before
addition of dye.
Effect of sequence of additions
The effect of sequence of additions on the oxidation process of nicotine was studied by
measuring the absorbance of solution prepared by different sequence of additions against a
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blank solution prepared in the same manner. Experiments showed that (Oxidant-Acid-Drug)
for both methods, gave the best results.
Effect of dye concentration
The optimum volume of dye used for production of maximum color intensity was 1.7 ml of
1.0 x 10-3 M (MO) for (method A), 1.6 ml of 1.0 x 10-3 M (AM) for (method B) Figure 4. The
effect of time after the addition of dye indicated that shaking for 1.0 min was sufficient to
give reliable results for all dyes. The color remains constant for at least 24 h.
Stoichiometric ratio
The stoichiometry of the reaction between nicotine and the oxidant at the selected conditions
was established by the molar ratio method. In this method 1.0 ml of 1.0 x 10-3 M NBS for
(method A), 1.0 ml of 1.0 x 10-3 M Ce(VI) for (method B) is kept constant and variable
concentrations (0.1 - 6.0 ml) of nicotine (1.0 x 10-3 M) were added using micropipette. The
absorbance was measured at λmax against blank solution prepared in the same manner. The
absorbance values were then plotted against the molar ratio [D]/[O]. The stoichiometry of
[D]/[O] at the selected conditions showed that the inflection of the two straight lines at 0.63
for (method A) 0.71 AM for (method B), Figure 6.
Reproducibility of the method
The reproducibility of the method was assessed by carrying out seven replicate analyses of a
solution containing 3.0 µg/ml of nicotine in a final solution volume of 25 ml. The standard
deviation and relative standard deviation of absorbance values were found to be ±0.011 and
0.56 %, respectively.
Analytical data
Beer's law was verified up to (0.1-4.8 µg/ml) for method A, and (0.3-5.9 µg/ml) for method B
as shown in (Figure 5) and Ringbom limits, molar absorptivities, Sandell sensitivities,
regression equations and correlation coefficients were calculated and recorded in (Table 1).
The limits of detection (K=3) and quantitation (K=10) were established according to IUPAC
definitions [40] are recorded in (Table 1).
In order to determine the accuracy and precision of the methods, solution containing three
different concentrations of nicotine were prepared and analyzed in six replicates (Table 2).
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0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
0.0 0.5 1.0 1.5 2.0 2.5 3.0
ml added of acid
Abs
orba
nce
NBSCerric
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
0.0 0.5 1.0 1.5 2.0 2.5 3.0
ml add of dyes
Abs
orpa
nce
MOAM
Fig. 3. Effect of ml added of acid (2.0 M HCl
using NBS, 2.0 M H2SO4 using Ce(VI));
nicotine (4.0 µg/ml), 1.1 ml of (1 x 10-3 M)
NBS, reaction temperature 80±1 °C; reaction
time: 4.0 min
Fig. 4. . Effect of ml added of dyes on
4.0 µg/ml nicotine, (MO in case of NBS,
AM in case of Ce(VI)), reaction
temperature 80±1 °C; reaction time:
4.0 min
Stability of colour
The pink or red colour formed was stable for at least 24 h under optimum conditions.
Validation method
The proposed method was successfully applied to determine nicotine in cigarettes tobacco
and in biological samples (spiked human plasma and urine). The accuracy of the proposed
methods is evaluated by applying standard addition technique, in which variable amounts of
the nicotine were added to the previously analyzed portion of extracted nicotine from
cigarettes tobacco and in biological samples (spiked human plasma and urine). The results
recorded in (Table 3), The results are in good agreement with those obtained by the reported
method [17-19], by Student’s t-test (for accuracy), and variance ratio F-test (for precision) [41],
at 95% confidence level as recorded in (Table 4). The results showed that the t- and F- values
were lower than the critical values indicating that there was no significant difference between
the proposed and reported methods. The proposed method was more accurate with high
recoveries.
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0.0
0.2
0.4
0.6
0.8
1.0
1.2
0.0 1.0 2.0 3.0 4.0 5.0 6.0 7.0
[D] µg ml-1
Abs
orba
nce
NBSCerric
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
0.0 0.5 1.0 1.5 2.0 2.5 3.0
[D]/[O]
Abs
orba
nce
NBSCe(VI)
Fig. 5. Calibration curve of nicotine µg/ml,
using NBS and Ce(VI) (1.0 x 10-3 M) and
dyes, MO and AM (1.0 x 10-3 M), reaction
temperature 80±1 °C; reaction time: 4.0 min
Fig. 6. Molar ratio method for nicotine
(1.0 x 10-3 M) using NBS and Ce(VI)
(1.0 x 10-3 M) and dyes, MO and AM
(1.0 x 10-3 M), reaction temperature
80±1 °C; reaction time: 4.0 min
Table 1. Optical and regression characteristics of nicotine for the proposed method.
Parameters
Proposed method NBS Ce(SO4)2
λmax (nm) 507 530 Stability / h 24 48 Beer’s law limits (µg/ml) 0.1 – 4.8 0.3 – 5.9 Ringbom limits (µg/ml) 0.3 – 4.5 0.6 – 6.3 Molar absorptivity (L/ mol.cm) 2.76 x 104 3.03 x 104 Sandell sensitivity (ng/cm2) 5.88 5.35 Detection limits (µg/ml) 0.058 0.052 Quantitation limits (µg/ml) 0.193 0.173 Regression equation a: Slope (b)
0.170
0.187
Intercept (a) 8.4 x 10-4 8.1 x 10-4 Correlation coefficient (r) 0.9996 0.9998 RSD b % 0.59 0.46 Calculated t-values (2.57) c 0.49 0.77 Calculated F-test (5.05) c 2.27 1.84 Stiochiometric ratio [D]/[O] 1.0 : 0.63 1.0 : 0.71
a A = a + bC where C is concentration of nicotine in µg/ml and A is absorbance.
b Relative standard deviation for six determinations. c Values in parentheses are the theoretical values for t- and F values at 95% confidence limits
and five degrees of freedom.
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Table 2. Evaluation of the accuracy and precision of the proposed procedures for
nicotine.
Reagent Taken µg/ml
Found µg/ml
Recovery %
RSD a %
RE b
% Confidence Limitsc
NBS
1.0 2.0 4.0
1.02 1.98 4.01
102.0 99.00 100.25
0.55 0.69 0.76
1.23 1.60 0.82
1.02 ± 0.0125 1.98 ± 0.0316 4.01 ± 0.0329
Ce(SO4)2
1.0 3.0 5.0
0.97 2.98 5.01
97.0 99.33 100.2
0.73 0.84 0.91
1.39 1.07 1.02
0.97 ± 0.0135 2.98 ± 0.0318 5.01 ± 0.0510
a Relative standard deviation for six determinations. b Relative error.
c 95% confidence limits and five degrees of freedom
Table 3. Determination of nicotine in cigarette tobacco in Libyan markets and biological
samples using standard addition technique.
Sample
Taken µg/ml
NBS Ce(VI) Added µg/ml
Found* µg/ml
Recovery %
Added µg/ml
Found* µg/ml
Recovery %
American Legend a
**
1.0
0.0 1.03 103.00 0.0 0.96 96.00 1.0 2.05 102.50 1.0 2.01 100.5 2.0 2.97 99.00 2.0 3.02 100.66 3.0 4.01 100.25 3.0 3.96 99.00
Marlloborro b **
1.0
0.0 0.97 97.00 0.0 0.98 98.00 1.0 2.05 101.00 1.0 2.07 103.5 2.0 2.99 99.00 2.0 2.96 98.66 3.0 3.96 99.50 3.0 3.99 99.75
Urine
1.0
0.0 0.98 98.00 0.0 1.01 101.0 1.0 1.98 99.00 1.0 1.96 98.00 2.0 2.97 99.00 2.0 2.95 98.33 4.0 4.03 100.75 4.0 4.07 101.75
Spiked human plasma
1.0
0.0 0.98 98.00 0.0 0.95 95.00 1.0 2.07 103.50 1.0 1.96 98.00 2.0 2.96 98.66 2.0 2.98 99.33 4.0 4.03 100.75 4.0 4.06 101.5
* Average of six determinations. ** Amount of sample: 0.1 gm. After treatment diluted to 50 ml, nicotine found in µg/ml of the
final solution. a Cigarette smoke, made in EU, under the authority of the Trade mark Owners, by KTG, INC.
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b. Cigarette smoke, Karelia light, Karelia tobacco company INC, made in Greece, nicotine
content o.7 mg.
Table 4. Determination of nicotine in cigarette tobacco in Libyan markets and in
biological samples using the proposed and reported methods.
Samples
NBS Ce(VI) Reported method[17] Recovery
% t-
test F-
value Recovery
% t-
test F-
value American Legend a * 98.80 1.22 2.49 97.77 0.82 2.33 96.55 Marlloborro b 99.17 0.89 1.99 98.97 0.99 1.87 98.71 Urine 97.89 1.08 2.07 98.10 1.16 2.24 97.07 Spiked human plasma 97.19 0.96 2.55 96.11 0.78 2.19 95.06
Theoretical value for t- and F- values for five degrees of freedom and 95% confidence limits
are 2.57 and 5.05, respectively.
* Amount of sample: 0.1 gm. After treatment diluted to 50 ml, nicotine found in µg/ml of the
final solution. a Cigarette smoke, made in EU, under the authority of the Trade mark Owners, by KTG, INC. b Cigarette smoke, Karelia light, Karelia tobacco company INC, made in Greece, nicotine
content o.7 mg.
CONCLUSION
The proposed method was advantageous over other reported visible spectrophotometric and
colorimetric methods, related to their high reproducibility, high sensitivity, less time
consuming and using simple and inexpensive reagents. Moreover, these methods allowed the
determination of nicotine up to 0.1 µg/ml, in addition to simplicity, rapidity, precision and
stability of colored species for more than 24 h.
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