Chebliislam@Live - FR: Orcid: Content Not Peer-Reviewed by Chemrxiv. License

Development and analytical validation of a method for the determination of lead, cadmium,
mercury and their isotopes in milk, honey, meat, fish and eggs by icp-ms
Authors: A.I. Chebli*,1, M.A. Reffai1, A. Amziane1,2, E. Shalabi3,H.Khan 4, J. Djerroud1, Y.

Zebbiche 2
Affiliations:
1: National center of toxicology, Algiers, Algeria
2: Faculty of pharmacy, university of Algiers 1, Algeria
3: college catholic, department of biochemistry, Canada
4: University of Waterloo, Belgium
* Email : chebliislam@live.fr , Tel : +213554777324 , ORCID : 0000-0001-9242-9733
Abstract
recent decades, industrial and urban development has been accompanied by real health problems
linked to environmental pollution and the contamination of foodstuffs of animal origin by heavy
metals such as lead, cadmium and mercury which are toxic to the immune, hematological, renal
and neurological system with a risk of developing cancer in the consumer of contaminated food.
The aim of this study was to develop and validate an analytical method to determine the metals
Cadmium (111Cd, 114Cd), Lead (208Pb) and Mercury (202Hg) in milk, honey, meat, fish and eggs
using inductively coupled plasma mass spectrometry (ICP-MS). For sample preparation,
microwave oven digestion with nitric acid and hydrogen peroxide is adopted.
The method showed linearity, accuracy and limits of quantification and detection acceptable for
LABGTA45 protocol validation of analytical methods in the area of food analysis.
Therefore, the method using ICP-MS was developed and validated to determine metals
concentrations in food matrixes and the proposed method could be applied in routine analytical
laboratory.
Key words-ICP-MS, Metals, Method validation, food matrixes
https://doi.org/10.26434/chemrxiv-2023-2ctkf ORCID: https://orcid.org/0000-0001-9242-9733 Content not peer-reviewed by ChemRxiv. License: CC BY-NC-ND 4.0
Introduction
The development of different types of metallurgical, automotive, material recycling and battery
manufacturing industries has been accompanied in recent decades by real health problems related
to environmental pollution (Başar S et al.2021, and Chebli A.I et al,.2022). Water, Air and soil
pollution remains the primary cause of contamination of animal food products such as fish, meat,
eggs, honey and milk (Guowei Qin et al.,2021 and Okoye EA et al.,2021 and Lu Y et al.,2015).
This poses a risk to the consumer, development of metabolic and endocrine disorders,
cardiovascular and renal disorders, development of different types of cancer, especially among
chronic consumers of these foodstuffs (Fernando Gil et al.,2021 and Sharma S et al.,2018 and Real
MIH et al.,2015)
The European Commission Regulation (EC) No 1881/2006 (Commission Regulation (EC) No.
1881/2006) sets a maximum level of contamination of heavy metals in food products (MRL) which
must not exceed 0.05 mg/kg in beef meat and fish meat for cadmium, 1 mg/Kg in fishery products
and 0.1 mg/Kg in beef meat for mercury, 0.3 mg/Kg in fish, 0.02 mg/Kg in milk and 0.1 mg/Kg
in honey for lead.
Like the other countries, Algeria has taken an interest in this problem in order to guarantee food
safety. Controls and surveillance devices for residues and contaminants in the food are put in place
(Radia zamoum et al.,2021, and Akli Islem Chebli et al., 2023).
The aim of this work is the development and the validation of an analytical method for the
determination of lead, cadmium and mercury and their isotopes in different food products of
animal origin. As well as the verification of the characteristics of the analytical method by the
evaluation of sensitivity, specificity, linearity, accuracy and repeatability using an inductively
coupled plasma mass spectrometry system (ICP-MS).
Material and method
1- Reagents and solutions
The different reagents used in this method of analysis are: standard Lead solution 1000mg/L
(PANREAC, Illinois USA), standard Cadmium solution 1000mg/L (PANREAC, Illinois USA),
standard Mercury solution 10000 mg/L (PANREAC, Illinois USA), Molybdenum standard
solution 1000mg/L (PANREAC, Illinois USA), Tungsten standard solution 1000mg/L
(PANREAC, Illinois USA), Indium internal standard solution 1000 mg/l (PANREAC, I llinois
USA), Rhodium internal standard solution 1000 mg/l (PANREAC, Illinois USA), Iridium Internal
Standard Solution 1000 mg/l (PANREAC, Illinois USA), Gold standard solution 100 mg/l
(PANREAC, Illinois USA), Daily check solution 1 µg/l containing Ba, Be, Bi, Ce, Co, In, Mg, Pb,
Th, Tl (Nexion , N8145051,PERKIN, USA) , Nitric acid HNO3 65 % (CARLO ERBA
V2A650182A,Italy),Hydrogen peroxide H2O2(30% V/V, ICP quality). The ultrapure water used
to prepare the standard solutions and samples is obtained from the milli-Q (Merck, Germany) water
production system (resistivity = 18.1 MΩ.cm). Solutions were prepared at different concentrations
(1:20 lead and cadmium solution, 1:200 mercury solution) for calibration range preparation and
quality checks. 1:100 solution prepared from internal standard solution. 1:10 solution prepared
from standard gold solution. Certified reference materials (CRM): DORM4 (National Research
Council of Canada).
2- Instrument
ICP-MS NexION® 300D (PerkinElmer Inc. USA) was used and operated with Nexion™ v1.5
software (PerkinElmer Inc. USA). The ICP is equipped with a concentric nebulizer (SilQ Plus
Quartz Nebulizer, N8152384), quartz cyclonic nebulizer chamber (N8152375) with controlled
temperature of -10°C to +80°C (PC3x Sample Introduction, N8152382), removable quartz torch
(Fixed SilQ 2 mm Torch, N8152428), Quartz Injector (2.0 mm Demountable Quartz Injector,
N8152376), Sampler, Skimmer and Hyper Skimmer Nickel Cones. A PerkinElmer Single Cell
Automation Kit for NexION (Single Cell Automation Kit), The autosampler was covered with a
clear acrylic casing to prevent contamination of the sample. The 99.9999% quality argon gas
(Linde gas. Algeria) is used for plasma. The ICP-MS NexION® is equipped with a dual-stage
detector (N8151011).
Acid digestion is performed through an Anton Paar Multiwave with 8-positions (Multiwave 5000,
Austria). equipped with a quartz microwave vessel.
3- Method
3-1- Sample preparation
The sample be heated to ambient temperature and homogenised before taking the test sample. The
purpose of the test samples is to get as close as possible to an equivalent of 0.20 to 0.25 g of dry
matter. In a quartz microwave vessel, the prepared samples are weighed; 2 g for fresh liquid
products like milk, 1 g for fresh products such as muscles, livers, fish, crustaceans, 0.5 g for honey,
eggs, and 0.20 to 0.25 g for dry or freeze-dried products.
Ultrapure distilled water is added to the freeze-dried products. Add 3 mL nitric acid solution. Leave
half hour in contact and add 0.5 mL of hydrogen peroxide and 2.5 mL of ultrapure H 2O. Wait at
ambient temperature for a minimum of 30 minutes for pre-digestion (EN 13805,2014). A digestion
blank is made in parallel (replacement of the test sample with 1 mL of ultra-pure water). Digestion
by microwave is initiated according to the digestion program presented in Table 1
The resulting digestate must be clear. A significant decrease in volume indicates that the container
was not hermetically closed. Cool the digestion vessel to ambient temperature. The resulting
solution is then transferred to a 50 mL tube (Eppendorf, Hamburg, Germany). 100 μL of the
internal standard solution is added before completing to volume with ultrapure water.
3-2- Instrumental method
Preheat the instrument in operation for a minimum of 30 minutes, and check the performance of
the instrument (sensitivity and stability of the system as well as the rate of oxides and double
charged ions) using the optimization Tunning solution. ICP-MS performance for the adopted
method is optimized and described in Table 2.
3-3- Quantitative Analysis
The linearity range, which indicates the range of concentrations where the instrument response is
proportional to the analyte concentration, is between [0.002-2] µg/g.
3-4- Validation method
The validation plan to define the characteristics and the implementation of the method for the
determination of heavy metals lead, cadmium, mercury and their isotopes in milk, honey, meat,
fish and eggs by ICP-MS, meets the technical accreditation guide LABGTA 45 (Lab GTA
45,2018) for the analysis of trace metal and mineral elements and their chemical species in
foodstuffs intended for human or animal consumption.
3-4-1-Linearity:
This experimental plan makes it possible to check the validity of the regression model, to check
the calibration domain and to deduce the characteristics. It also allows to define a working area
according to NF T90210 (NF T90-210,2013). Five calibration levels included in the supposed
domain. 5 calibration ranges under intermediate fidelity conditions and measure the information
value.
The study of calibration in the chosen domain can be interpreted by an individual verification
approach in relation to a maximum acceptable deviation (MAD calibration). The aim is to verify
that the differences observed on each standard analyzed (% residual deviation between the
theorical and the calculated value on the linear model) are acceptable in relation to a calibration
MAD set by the laboratory for each standard.
3-4-2-Sensitivity, detection and quantification limit:
To determine the detection limit (LOD) and quantification limit (LOQ), 21 blank tests are analyzed
under internal reproducibility conditions according to NF13804 (EN 13804,2013). After
verification of the absence of possible aberrant points (Shapiro-Wilk Test) the detection limit is
numerically equal to 3 times the standard deviation, and the quantification limit is numerically
equal to 10 times the standard deviation of the mean of the blank tests. The blank test consists of
fish, milk, egg, honey and meat matrix free of heavy metals.
3-4-3-Specificity:
The study of the matrix effect or non-specific interference is based on the evaluation of the
recovery according to the charge of the matrix, the calculation of the recovery by the measurement
of the intensities of lead, cadmium, mercury in charged matrix at different levels [0.1-2] g.
The study of the effect of the salts is also carried out by preparing an increasing range of saturated
solution in sodium chloride (NaCl) [1-50] g, charged with a concentration of 100 µg/L in lead,
cadmium, mercury isotopes, the study consists of evaluating the drift of the signal obtained.
3-4-4-Repeatability and Accuracy (Accuracy Profile):
The accuracy study focuses on the evaluation of intermediate fidelity and bias against values that
serve as a reference according to NF V03-110 (NF V03-110,2010). The accuracy of the method is
checked on samples of reference values and according to a maximum acceptable deviation from a
regulatory or normative requirement (15%). The accepted reference value is provided by the
certificate value of a Certified Reference Material (CRM) or by adding the analyte to a matrix
representative of the application area.
The organisation of the tests consists of preparing at least three samples covering the field of
application of the method. Analyse each sample in at least 5 series under conditions of intermediate
fidelity. Carry out at least 3 concentration levels (level 1: LQ, level 2: MRL, level 3: 10 times
MRL) covering the linearity domain of the method. For each sample and in each series, perform
at least 2 repeats under repeatability conditions.
3-4-5-Uncertainty calculation:
The standard deviation of intermediate fidelity for each level measured under conditions of
intermediate fidelity is the standard uncertainty of fidelity (Uc). The extended uncertainty U is
obtained by multiplying the standard uncertainty by a factor k (k=2) called the coverage factor,
which makes it possible to obtain an interval corresponding to the confidence level of about 95%
according to ISO 11352 (ISO 11352,2012)
Results and discussion
The ICP-MS system performance check is performed by injecting a certified solution specified by
the manufacturer PerkinElmer. This procedure was used to evaluate the equipment and its
sensitivity and the percentage of cerium oxides (CeO/Ce) that should be < 0.025 . The supplier
recommends intensities for the elements Be > 5000 , Mg > 25000, In > 70000 and U > 50000, the
rate of doubly charged elements is evaluated by measuring the intensities of Ce++ . Optimal results
are shown in Table 3.
Linearity and Calibration:
The normality test is verified by the Shapiro Wilk test, the observed value W must be greater than
the critical values W limit to 5% to declare a normal distribution, after checking the normality of
the data, the results conclude that the data follow a normal distribution.
The validation of the calibration model is carried out by evaluating the distribution of residues in
% according to the levels related to the MAD defined by the laboratory, the following Table 4
summarizes the distribution of relative residues in relation to the theoretical quantities.
All levels of validation for Pb208, Cd111, Cd114 and Hg202 fall within the MAD domain under
the conditions of repeatability, The % distribution of residues according to levels relative to MAD
meet the requirements of NF T90210.
Detection and quantification limit:
The detection and quantification limits calculated on 21 matrix blanks, the LOD concentration (3σ
blank) and LOQ concentration (10σ blank) are evaluated after checking the normality of the
distribution, the results obtained from the LOD and LOQ are represented in Table 5.
The limit of quantification of Cd, Pb, Hg meets the standard NF13804, the limit of quantification
of cadmium is less than 1/6th of the lowest MRL, for mercury its limit of quantification is less
than 1/5th of the lowest MRL, and for lead the limit of quantification is less than ½ of the lowest
MRL.
Accuracy profile
the evaluated accuracy profile on 3 validation levels is interpreted compared to the lower and
higher acceptance limit, the results are presented in Table 6.
The percentage of recovery of Cd 111, Cd 114, Hg 202, Pb 208 in meat products, fishery products,
milk, eggs and honey, against acceptance limit are shown in Figure 1-5.
Figures (1-5) show that the tolerance interval is included in the acceptability interval, it can be
concluded that the method is valid in the field studied and this for all isotopes in all matrices.
No tolerance limit is outside the acceptability limit, therefore, the method is provided sufficient
acceptable results, depending on the criteria chosen
Uncertainty factor
Uncertainty estimation with ISO 11352 (29) is shown in Table 7.
The results meet the requirements of the standard. The results show that for the lowest level the
measurement uncertainty ranges from 32% for lead to 52% for mercury, for other levels the
measurement uncertainty does not exceed 30%.
Conclusion
A method using ICP-MS has been developed and validated to determine the level of heavy metals
lead, cadmium and mercury in foodstuffs of animal origin (meat products, fishery products, milk,
eggs, honey). The method showed acceptable linearity, repeatability, accuracy, LOD and LOQ
according to the proposed validation protocol. These parameters ensure that the proposed
methodology could be applied in routine analytical laboratories.
Conflicts of interest
The authors declare that they have no conflicts of interest in relation to this article.
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https://doi.org/10.1007/s12011-023-03891-x
12- EN 13805. (2014) Foodstuffs - Determination of trace elements by Pressure digestion.
AFNOR guideline .
13- Lab GTA 45. (2018) Analysis of metallic trace elements and minerals and their chemical
species in the food for human consumption or animals. Cofrac guideline version 2. 2021
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validation and quality control.
list of figures and tables
Figure 1: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in meat products

Red: limit of acceptability%, green: tolerance limit %, blue: recovery %
Figure 2: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in fishing products
Figure 3: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in Milk
Figure 4: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in Eggs
Figure 5: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in Honey
Table 1: Microwave Digestion Program

STEPS POWER RAMP LEVEL COOLING
(W) (MIN) (MIN) SPEED
1 500 0 1 1
2 800 10 0 1
3 1000 10 0 1
4 0 0 20 3
Table 2: Instrumental performance
PARAMETER SETTING
MODE Standard
INTRODUCTION SYSTEM: Analyse: 24 rpm
PERISTALTIC PUMP Read delay: 24 rpm
Wash: 34 rpm
Flush: 30 rpm
GENERATOR Incident power: 1300 W
Reflected power: < 5 W
GAS FLOW RATES Plasma : 15 L/min
Nebulization: 1.2 L/min
Auxiliary: 1.1 L/min
SCAN Mode: peak Hopping
Integration time (ms): 1000
ACQUISITION PARAMETERS Channels: 1
Replicates: 3
Sweep/replicate: 20
RP: 0.25
Dwell time (ms): 50
TIME Reading time (s): 15
Replicate time (s): 15
Sample training time (s): 45
ISOTOPES 111Cd and 114Cd
202Hg
206Pb, 207Pb, 208Pb
EQUATION OF CORRECTION Cd 111= - 0.0047 x Mo98
Cd 114= -0.027 x Sn 118
Mo 98 = -0.11 x Ru 101
Hg 202 = -0.003 x W 183
INTERNAL STANDARD Rh
Table 3: tuning result
PARAMETERS SIGNAL
BE 9.0122 > 5000
MG 23.985 > 25000
IN 114.904 > 70000
U 238.05 > 50000
CEO 155.9 >0
CE 139.905 >0
CE++ 69.952 <0
BACKGROUND <1
CEO 155.9/ CE 139.905 < 0.025
CE++ 69.952/ CE 139.905 < 0.03
Table 4. Table of relative residues in relation to theoretical quantities
Repetition 1 2 3 4 5 Average MAD MAD
Levels
Pb 208 -14.46% 15.71% -5.22% 12.31% -18.6% -6.07%
Level 1= Cd 111 -12.14% 0.65% 17.94% -15.7% 17.07% -2.44%
20.00% -20.00%
0.002 µg/g Cd 114 -10.88% 19.26% 2.18% 2.71% 9.59% -3.43%
Hg 202 -16.11% -2.60% 15.64% -14.2% -13.4% -8.16%
Pb 208 -7.94% 0.59% 0.65% 12.15% -19.9% -2.90%
Level 2= Cd 111 -12.62% -3.33% 7.05% -0.61% 10.08% -1.88%
10.00% -10.00%
0.005 µg/g Cd 114 -13.96% 2.47% 1.08% 6.87% 9.52% -2.80%
Hg 202 -18.83% -4.82% 5.30% 1.19% -1.03% -3.64%
Pb 208 -5.01% 1.19% 1.71% 0.88% -3.04% -0.85%
Level 3= Cd 111 -4.18% 2.67% -1.68% -0.80% -0.40% -0.88%
10.00% -10.00%
0.2 µg/g Cd 114 -4.78% 3.59% -0.13% -0.84% 1.22% -0.19%
Hg 202 -3.12% 1.21% -3.87% 2.21% 1.25% -0.46%
Pb 206 3.11% -0.02% -0.82% -1.63% 2.75% 0.68%
Level 4= Cd 111 6.19% 0.17% -0.98% -0.30% 1.28% 1.27%
10.00% -10.00%
0.5 µg/g Cd 114 8.54% -0.71% -0.32% 0.35% 1.21% 1.81%
Hg 202 6.07% 0.48% -2.35% 0.05% 2.95% 1.44%
Pb 208 0.82% -1.89% 0.14% -2.93% 5.46% 0.32%
Level 5= Cd 111 0.34% -0.79% -0.06% 1.19% -2.47% -0.36%
10.00% -10.00%
1 µg/g Cd 114 0.64% -1.76% 0.10% -0.74% -2.66% -0.88%
Hg 202 -0.95% -0.22% 1.23% 0.01% -1.24% -0.23%
Pb 208 -0.34% 0.46% 0.00% 0.81% -1.48% -0.11%
Level 6= Cd 111 -0.41% 0.16% 0.09% -0.27% 0.53% 0.02%
10.00% -10.00%
2 µg/g Cd 114 -0.62% 0.45% 0.00% 0.17% 0.57% 0.11%
Hg 202 -0.10% 0.02% -0.13% -0.03% 0.12% -0.02%
Table 5: LOD LOQ values for Cd, Pb, Hg in meat, fish, milk, egg and honey
isotopes LOD µg/kg LOQ µg/kg

Cd 111 0.0006 0.0019
Cd 114 0.0005 0.0016
Hg 202 0.0006 0.0019
Pb 208 0.0004 0.0013
Table 6: Representation of Cd 111, Cd 114, Hg 202, Pb 208 Accuracy Profile Data in meat products, fishery products, milk, eggs and honey
Criteria Level 1 Level 2 Level 3

ISOTOPE Cd 111 Cd 114 Hg 202 Pb 208 Cd 111 Cd 114 Hg 202 Pb 208 Cd 111 Cd 114 Hg 202 Pb 208
AVERAGE 0.022 0.021 0.022 0.022 0.053 0.021 0.051 0.053 0.815 0.817 0.765 0.755
CONCENTRATION
RECOVERED
REFERENCE VALUES 0.02 0.02 0.02 0.02 0.05 0.02 0.05 0.05 0.81 0.81 0.75 0.75
RECOVERY % 108.14 103.02 112.01 109.42 105.25 103.02 101.10 105.98 100.97 101.29 101.98 100.69
LOW TOLERABLE 0.018 0.018 0.015 0.019 0.044 0.018 0.037 0.041 0.713 0.713 0.606 0.672
LIMIT
HIGH TOLERABLE 0.023 0.023 0.029 0.025 0.059 0.023 0.064 0.065 0.922 0.922 0.923 0.838
LIMIT
LOW LIMIT IN % 90.24 90.24 77.27 95.65 88.72 90.24 73.83 82.36 88.31 88.31 80.83 89.66
HIGH LIMIT IN % 115.79 115.79 146.75 123.19 118.77 115.79 128.37 129.61 114.27 114.27 123.12 111.71
LOW ACCEPTABLE 0.008 0.008 0.008 0.008 0.035 0.008 0.035 0.035 0.565 0.565 0.525 0.525
LIMIT
HIGH ACCEPTABLE 0.032 0.032 0.032 0.032 0.065 0.032 0.065 0.065 1.049 1.049 0.975 0.975
LIMIT
LOW ACCEPTABLE 40.00 40.00 40.00 40.00 70.00 40.00 70.00 70.00 70.00 70.00 70.00 70.00
LIMIT %
HIGH ACCEPTABLE 160.00 160.00 160.00 160.00 130.00 160.00 130.00 130.00 130.00 130.00 130.00 130.00
LIMIT %
Tables 7: relative uncertainty by element and by matrix
Element Relative Uncertainty (%)

level 1 level 2 level 3
Meat product
Cd 111 33.59 16.74 9.64
Cd 114 26.50 16.67 10.43
Hg 202 52.00 22.25 15.99
Pb 208 32.21 24.00 9.39
Fishery product
Cd 111 33.89 19.41 11.24
Cd 114 20.44 22.90 6.27
Hg 202 20.80 22.24 12.24
Pb 208 20.76 27.67 14.80
Milk
Cd 111 25.31 19.48 10.27
Cd 114 26.67 21.83 15.16
Hg 202 33.64 21.96 12.81
Pb 208 42.66 25.67 7.80
Eggs
Cd 111 27.52 26.44 11.12
Cd 114 26.08 28.31 18.59
Hg 202 47.76 28.76 16.37
Pb 208 36.92 29.37 14.86
Honey
Cd 111 25.71 20.53 16.48
Cd 114 24.68 21.45 16.13
Hg 202 32.64 20.56 17.25
Pb 208 33.53 23.17 19.95

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Development and analytical validation of a method for the determination of lead, cadmium,

Authors: A.I. Chebli*,1, M.A. Reffai1, A. Amziane1,2, E. Shalabi3,H.Khan 4, J. Djerroud1, Y.

Key words-ICP-MS, Metals, Method validation, food matrixes

Material and method

1- Reagents and solutions

3-1- Sample preparation

3-2- Instrumental method

3-3- Quantitative Analysis

3-4- Validation method

3-4-2-Sensitivity, detection and quantification limit:

3-4-4-Repeatability and Accuracy (Accuracy Profile):

Results and discussion

Linearity and Calibration:

Detection and quantification limit:

Uncertainty estimation with ISO 11352 (29) is shown in Table 7.

Figure 1: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in meat products

Figure 2: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in fishing products

Figure 4: recovery percentage of Pb 208, Hg202, Cd 111, Cd114 in Eggs

Table 1: Microwave Digestion Program

isotopes LOD µg/kg LOQ µg/kg

Cd 114 0.0005 0.0016

Hg 202 0.0006 0.0019

Pb 208 0.0004 0.0013

Criteria Level 1 Level 2 Level 3

Element Relative Uncertainty (%)

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