Agricultural Research Management Information System

Home
Research Summary
Search
About Us
- ARMIS
- Brochure
Contact Us
Report
User Request
Data Input
Help
- Operation Manual
  - PDF
  - Video
- Program Area & Commodity
We have reached 37600 number of research entries at this moment.

- Logout

Research Detail

Home
Research
Detail

Development and Validation of a Gf-aas Method and Its Application for the Trace Level Determination of Pb, Cd, and Cr in Fish Feed Samples Commonly Used in the Hatcheries of Bangladesh

A. K. M. Atique Ullah
Analytical Chemistry Laboratory, Chemistry Division, Atomic Energy Centre, Bangladesh Atomic Energy Commission, Dhaka 1000, Bangladesh

M. A. Maksud, S. R. Khan
Analytical Chemistry Laboratory, Chemistry Division, Atomic Energy Centre, Bangladesh Atomic Energy Commission, Dhaka 1000, Bangladesh

L. N. Lutfa
Analytical Chemistry Laboratory, Chemistry Division, Atomic Energy Centre, Bangladesh Atomic Energy Commission, Dhaka 1000, Bangladesh

Shamshad B. Quraishi
Analytical Chemistry Laboratory, Chemistry Division, Atomic Energy Centre, Bangladesh Atomic Energy Commission, Dhaka 1000, Bangladesh

Abstract/ Executive Summary:

Background

A sensitive, accurate and precise method was developed and validated in regard to Council Directive 333/2007/EC, Commission Decision 657/2002/EC, ISO/IEC 17025:2005 and EURACHEM 1998 for the trace level determination of Lead (Pb), Cadmium (Cd) and Chromium (Cr) in fish feed samples using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS).

Methods

For method validation, selectivity, working and linear ranges, limit of detection (LoD), limit of quantification (LoQ), trueness (recovery) and precision (repeatability and reproducibility) have been assessed as performance criteria.

Results

The method LoDs for Pb, Cd and Cr were found to be 0.078, 0.010 and 0.022 μg/g respectively, whereas, the method LoQs were obtained at 0.156, 0.021 and 0.044 μg/g respectively. Moreover, the recovery of the analytes was 90 – 104% and the RSD values for precision were 4.90 – 9.60% respectively.

Conclusions

The method validation performance criteria indicate the method’s suitability for trace level quantification of Pb, Cd, and Cr in fish feed samples.

Keywords: GF-AAS method, Pb, Cd, Cr, Fish feed, Hatcheries, Bangladesh

Location: Bangladesh

Start Date:

End Date:

Program Area: Risk Management in Agriculture

Commodity: Health hazard, Fish

Objectives:

This is the first attempt to quantify the toxic metals, Pb, Cd, and Cr, in fish feed samples widely used in the hatcheries of Bangladesh using a validated analytical method.

Methodology:

Instruments and reagents

A Varian AA280Z atomic absorption spectrometer with Zeeman background correction system equipped with a graphite furnace (GTA 120) and an autosampler (PSD 120) was used. The purity of argon gas was 99.999%. Hollow cathode lamps were used for Pb (283.3 nm and slit 0.5 nm), Cd (228.8 nm and slit 0.5 nm), and Cr (357.9 nm and slit 0.2 nm) and operated according to the conditions recommended by the manufacturer. Atomic signals were measured in peak area mood. The digestions were performed using a microwave oven (MARS’5, CEM Corporation, USA).

The bulk standard solutions 75 μg_PbL⁻¹, 6 μg_cdL⁻¹, and 20 μg_crL⁻¹ were daily prepared by appropriate dilution of 1000 μgL⁻¹ Pb, Cd, and Cr stock standard solutions respectively using 1% (w/w) Suprapur grade nitric acid (Merck, Darmstadt, Germany). The working standard solutions were prepared automatically by the autosampler from bulk standard solution. Phosphoric acid (H₃PO₄; Merck, Darmstadt, Germany) and ammonium phosphate monobasic (NH₄H₂PO₄; Merck, Darmstadt, Germany) were used as chemical modifiers for the determination of Pb and Cd, respectively. The reagents were all of analytical grade, and all solutions were prepared using deionized water (18 MΩ/cm) produced using an E-pure system (Thermo Scientific, USA). All containers and glassware were cleaned by soaking into 20% (w/w) nitric acid for at least 24 h and rinsed three times with deionized water prior to use.

Sample preparation

One gram of the homogenized fish feed samples was weighted into the polytetrafluoroethylene digestion vessel, and 6 mL of Suprapur nitric acid was added. Subsequently, the samples were digested with the microwave oven using a two-step temperature program. During the first step, the temperature was linearly increased to 180 °C for 10 min, the maximum power of the rotating magnetron was 1600 W. During the second step, the temperature was maintained at 180 °C for 15 min. After digestion and cooling, each solution was diluted to a final volume of 10 mL with deionized water.

Quality control programs

Internal quality control charts (IQCs) were also constructed in order to monitor whether results are reliable enough to be released. The objective of IQCs is the elongation of method validation: continuously checking the accuracy of analytical data obtained from day to day in the laboratory. The analytical system is under control if no more than 5% of the measured values exceed the warning limits and none of them the action or control limits. The external quality assurance program was maintained through the participation in proficiency programs organized by Asia Pacific Metrology Program-Asia Pacific Laboratory Accreditation Cooperation (APMP-APLAC) and LGC, UK. The results of proficiency tests were within ±2 Z scores.

Source of Information: Journal of Analytical Science and Technology volume 8, Article number: 15 (2017)

Article Link (Online Journal): DOI 10.1186/s40543-017-0124-y

Funding Source:

Budget:

Total Budget (Tk.) :

Achievement/Findings:

The current work describes the development and validation of a method for the trace level analysis of Pb, Cd, and Cr in fish feed in regard to Council Directive 333/2007 EC, ISO/IEC 17025:2005, and EURACHEM 1998 using Graphite Furnace Atomic Absorption Spectrometry (GF-AAS). The validation results are presented and organized in tables in order to provide an easy overview of the method’s performance. The validation data show that the present developed method has met all acceptance criteria defined in 657/2002/EC and 333/2007/ EC for LOD, LOQ, accuracy, and precision, and fit for the analysis of Pb, Cd, and Cr in fish feed at a very low level (μg/g). The method was implemented in routine analysis in order to investigate the fish feed quality commonly used in the hatcheries of Bangladesh. The results indicated that the elemental contents were lower than the legislative values, as described by the Council Directive 2002/32/EC concerning undesirable substances in animal feed.

Knowledge Management: Journal