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Confirmation of Chloramphenicol in Fish Feed (maize Flour) by Lc/ms-ms

M. A. Parvez
Technologist, Fish Inspection & Quality Control Laboratory, Matshya Bhaban, Ramna, Dhaka, Bangladesh

M. A. Alam
Biochemist, Fish Inspection & Quality Control Laboratory, Matshya Bhaban, Ramna, Dhaka, Bangladesh

M. S. Islam
Technical Manager, Fish Inspection & Quality Control Laboratory, Matshya Bhaban, Ramna, Dhaka, Bangladesh

M. M. Mia
Quality Manager, Fish Inspection & Quality Control Laboratory, Matshya Bhaban, Ramna, Dhaka, Bangladesh

M. B. Hossain
Quality Control Officer, Fish Inspection & Quality Control Laboratory, Matshya Bhaban, Ramna, Dhaka, Bangladesh

Abstract/ Executive Summary:

Maize flour is the most common item that has been used as fish feed. Due to locally available, cheap and highly productive feed for fish, maize flour has been used by the farmers. To protect from some diseases, chloramphenicol is used in fish feed illegally. This paper focus on the confirmation of chloramphenicol in fish feed by developing method and validated it in maize flour matrix by LC-MS/MS, which is important for maintaining the quality of fish feed. The monitored MRM transitions for CAP were m/z 321.1416 151.5853 and m/z 321.1416 257.0155 and for CAP_D5 was m/z 326.1416 156.81. Limit of decision (CCα) was 5.63µg/kg and detection capability (CCβ) was 9.57µg/kg.

Keywords: Confirmation, Chloramphenicol, Fish feed, Maize flour, LC/MS-MS

Location: Fish Inspection & Quality Control Laboratory, Matshya Bhaban, Ramna, Dhaka, Bangladesh

Start Date: 00-01-2002

End Date: 00-08-2002

Program Area: Postharvest and Agro-processing

Commodity: Feed

Objectives:

1. This study comprises the analysis chloramphenicol in fish feed(Maize flour), method was validated as per Commission Decision 2002/657/EC of 12 August 2002 implementing Council Directive 96/23/EC establishes criteria and procedures for the validation of analytical methods to ensure the quality and comparability of analytical results generated by official laboratories.

Methodology:

Sample Preparation: Standards and Reagents: Chloramphenicol (98%) and Chloramphenicol D5 (97%) as internal standard was purchased from Sigma-Aldrich(st. Louis, MO). MS grade methanol and acetonitrile were also from Sigma-Aldrich(st. Louis, MO).Beside these HPLC grade chemicals (Ethyl acetate, N-Hexane, Acetonitrile, Methanol) and Sodium Chloride, Phosphate buffered saline were used. 1- Weigh portions (3 ± 0.05) g (Dry basis) of maize flour into 30 ml screw capped glass boiling tube. 2- Include negatives and recoveries, present negative samples for QA. 3- Add 900 µl of 100 ppb D5-CAP working internal standard solution to all tubes. 4- Allow to stand for 10 min. 5- Add 4 ml PBS . 6- Add 1 ml of sodium chloride solution and mix for 1 min. 7- Add 4 ml of acetonitrile, vortex for 1 min. 8- Centrifuge @ 5000 rpm for 20 min. 9- Transfer supernatant to a clean 50 ml centrifuge tube. 10- Add 10 ml deionized water. 11- Add 10 ml hexane and shake gently for 30 sec. 12- Centrifuge the tubes @ 5000 rpm for 20 min and discard the upper hexane layer. 13- Add 8 ml of ethyl acetate. 14- Mix by vortex for 1 min. 15- Centrifuge the tubes @ 5000 rpm for 20 min. 16- Transfer organic solvent layer (upper layer) to glass tubes and take to dryness at 65 0C under nitrogen gas. 17- Reconstitute residue in 5 ml deionized water. Clean-up/SPE: Manual SPE: All columns and collection tubes are clearly labeled. All solutions are passes all through SPE columns under gravity. Set up vac box and vacuum pump. Varian C18 columns are good sealed between column and needle. Confirmation criteria:The selectivity of this method is judged by the use of two transitions for each analyte which count for 4 identification points (IPs), as defined by the EU criteria set out in Commission Decision 2002/657/EC. Our method fulfils this requirement. The Chloramphenicol was considered as positively identified in the samples when the peak area ratio of the various transitions was within the tolerance set by Commission Decision 2002/657/EC. In addition, the relative retention time of the analyte must be equal to that of the calibration standard to within ± 2.5%. Validation: CCα & CCβ were calculated using the procedure set out in ISO Guide 11843, as described in Commission Decision 2002/657/EC. The validation data were generated in 3 levels of concentrations i.e. 15ppb, 30ppb, 45ppb with seven replicates per level for 3 different days using maize flour as matrix.

Source of Information: Journal of Agricultural Engineering, The Institution of Engineers, Bangladesh, Vol. 41/AE Number 1, June, 2014

Article Link (Online Journal):

Funding Source:

Total Budget (Tk.) :

Achievement/Findings:

The method was developed and validated as per guideline and commission decision 2002/657/EC. The validation data provides the values CC =5.63 g/kg and CC =9.57 g/kg in Maize flour (Fish Feed). The recovery, linearity and other parameters explains that the developed method is good enough for the confirmatory analysis of CAP by LC/MS-MS in Maize flour(Fish Feed) matrix.

Knowledge Management: Journal