scholarly journals Method modified AOAC 2015.01 in the microwave conditions and the addition of HCl during sample digestion for simultaneous Pb, Cd, Hg, and As in infant formula using ICP-MS: a method validation

Food Research ◽  
2021 ◽  
Vol 5 (6) ◽  
pp. 211-220
Author(s):  
I.S. Maulidyah ◽  
D.N. Faridah ◽  
H.N. Lioe

The presence of heavy metals in infant formula has become a global concern. The most common method to determine heavy metals is AAS. However, as this technique is lacking in several aspects, including the instrument’s low sensitivity, a more sensitive instrument such as ICP-MS is necessary. The Inductively Coupled Plasma Mass Spectrometry (ICPMS) was used in accordance with the standard method AOAC 2015.01 with modifications on the microwave condition and the addition of hydrochloric acid (HCl) during the sample digestion process. The modified standard method requires a validation process. This research aimed to validate the method of analysis for the determination of Pb, Cd, Hg, As in infant formula using ICP-MS and its application in formula milk. This research consists of five stages: 1) instrumental performance; 2) homogeneity test; 3) method orientation; 4) method validation; and 5) the application of the validated method to other products. The findings in the research were: the method linearity was confirmed at working concentration 5-30 µg/kg for all the heavy metals with R2 value of nearly 1,000; the method limits of detection (LOD) were 0.74 µg/kg (Pb), 0.41 µg/kg (Cd), 0.08 µg/kg (Hg), 0.50 µg/kg (As), while the method’s limits of quantification (LOQ) were 2.48 µg/kg (Pb), 1.36 µg/kg (Cd), 0.27 µg/kg (Hg), 1.67 µg/kg (As); the method was found precise with Relative Standard Deviation (RSD) below 2/3 RSD Horwitz and all the recovery values were found to fall within the acceptable range (60–115%); the % RSD intra-lab reproducibility was below RSD Horwitz; and the method was robust, indicating that it was unaffected by small changes in its variables. The validated method can be applied routinely to determine heavy metals in infant formula and formula milk.

2017 ◽  
Vol 37 (1) ◽  
pp. 79-86 ◽  
Author(s):  
Saeed Akhtar ◽  
Muhammad Arif Shahzad ◽  
Sang-Ho Yoo ◽  
Amir Ismail ◽  
Aneela Hameed ◽  
...  

2020 ◽  
Vol 103 (5) ◽  
pp. 1282-1287
Author(s):  
Tamer M A M Thabit ◽  
Dalia I H Elgeddawy ◽  
Shokr Abdelsalam Shokr

Abstract Medicinal herbs are the ancient, traditional way of treating many diseases and are now considered the first natural source of pharmaceutical active ingredients. Therefore, it is very important to focus on the hygiene of these plants so as to make sure they are safe for consumption. This work aimed to monitor the common heavy and radioactive elements in some commonly used herbs: anise, chamomile, clover, cumin, coriander, fennel, roselle, rosemary, sage, and thyme. A total of 12 elements were measured including 2 radionuclides, Al, As, Cd, Hg, Co, Cr, Ni, Pb, Sr, Th, U, and V. Heavy metals are ecologically and biologically important, and may be involved in some health disorder symptoms within the human body. Samples were digested with a microwave digester and measurements were completed with ICP-MS/MS in Helium mode to increase sensitivity, lower the background, and avoid interferences. Method validation and verification were performed through the spiking process at 2.0 µg/kg level, and then RSD, LOD, and LOQ were calculated. Recoveries ranged from 93–103% for all elements and RSD% from 2.8–9.6%. Hg and Th were not detected in all samples, while U was detected in some sample of anise, rosemary, sage, and thyme, and ranged from 0.018–0.048 mg/kg. As was detected in anise, fennel, roselle, and rosemary, and ranged from 0.0.031–5.88 mg/kg. Al, Cd, Co, Cr, Ni, Pb, Sr, and V were detected in most samples of all herbs, and ranged from 3.88–17.80, 0.122–0.654, 0.019–0.851, 0.344–2.91, 1.872–5.82, 0.120–12.56, 0.128–0.844, and 0.083–0.912 mg/kg, respectively.


2019 ◽  
Vol 85 (6) ◽  
pp. 11-24
Author(s):  
I. V. Nikolaeva ◽  
A. A. Kravchenko ◽  
S. V. Palessky ◽  
S. V. Nechepurenko ◽  
D. V. Semenova

Two methods — ICP-MS and ICP-AES are used for certification of the new reference material — needles of Siberian pine (NSP-1). Techniques of the analysis include decomposition of plant samples in two different ways: acid digestion in a microwave system MARS-5 and lithium metaborate fusion followed by ICP-MS and ICP-AES analysis of the solutions. Simultaneous determinations of all the elements were carried out in low, medium and high resolution using SF-mass-spectrometer ELEMENT and atomic-emission spectrometer IRIS Advantage with external calibrations and internal standards (In — ICP-MS, Sc —ICP-AES). Middle and high resolutions of ICP mass spectrometer were used for interference corrections. Data obtained by ICP-MS and ICP-AES with different decomposition techniques are in good agreement. The ICP-MS and ICP-AES techniques have been validated by the analysis of three plant reference materials: LB-1 (leaf of a birch), Tr-1 (grass mixture) and EK-1 (Canadian pondweed). These techniques were used for the determination of 38 elements in the new reference material NSP-1. Relative standard deviations for most of the determined elements were below 10%. Combination of ICP-MS and ICP-AES techniques for certification of the new reference material makes it possible to expand the set of elements to be determined and to reduce the total analysis time.


Infant’s feeding patterns are important for development and growth; therefore babies are very sensitive to toxic elements, mainly through their food, so in the present study, the concentrations and daily intake of some Toxic Elements (TEs); Lead (Pb), Arsenic (As), Cadmium (Cd), Mercury (Hg) and Aluminum (Al) were measured in different and random 60 dried infant foods {30 infant formula (0-6 months) and 30 milk-cereal based infant formula (6 months)} which obtained from various supermarkets and pharmacies. The analysis was done using Inductive Coupled Plasma - Mass Spectrometer (ICP-MS). It could be determined the lead, arsenic, cadmium, mercury and aluminum by mean values of 0.424±0.006, 0.205±0.003, 0.014±0.0001, 0.298±0.007and 0.464±0.029 mg/Kg in the examined infant milk formula samples and a ranged minimum to maximum concentrations of 0.114-0.177, 0.155-0.293, 0.014-0.015, 0.282-0.310 and 0.287-0.437 mg/kg, respectively in the examined milk-cereal based infant formula. Present study indicates that, the greater level of contamination of examined infant formula samples with toxic elements (lead and mercury) surpasses the maximum limit and Provisional Tolerable Daily Intake (PTDI) of these elements. Mercury is over PTDI (0.0005 mg/kg bw/day) in all milk-cereal based infant formula samples, also arsenic in all examined samples of this type of formula was exceed the maximum limit (0.05 mg/kg) of Indian standard. This investigation shows such types of infant formula need more amendment to set limit of more toxic metals for this sensitive group of population.


Author(s):  
Yahya R. Tahboub ◽  
Adnan M. Massadeh ◽  
Nihaya A. Al-sheyab ◽  
Diab El shrafat ◽  
Israa A. Nsserat

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