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PESTICIDE RESIDUE ANALYSIS

IN LABORATORY
Jaminan Mutu Hasil Pengujian
1 : Kualifikasi
instrumen =
Membuktikan kelayakan
instrumen

2 : Validasi Metode
Analisis =
Membuktikan kelayakan
prosedur analisis

3: Sistem Suitability
Test = Verifikasi
Panduan dalam Metode Analisis
Dan Validasi Metode

Fisika-Kimia (Food and Pharmacy) : ICH, USP,


AOAC, FDA, EURACHEM, ISO, CDER, EMEA,
BPOM

Bioanalisis : FDA, EMEA

Pesticide : SANCO/SANTE (EU), EPA


Bahaya Pestisida bagi kesehatan

Neurotoxicant : Lindane, Aldrin, dieldrin, endrin


Carcinogen : Aldrin, BHC
Mutagen : Endosulfan
Endocrine Disrupter : Methoxychlor

Batas maksimum Residu Pestisida = MRL


(Maksimum Residual Limits) ditetapkan oleh
WHO, FAO dan EC
Contoh
Prosedur
Penetapan
Residu
Pestisida
dalam Apel

(Agilent
Method)
Metode Quantitasi dalam MS

External Calibration: Satu konsentrasi standar (


C sample +/- 30% dari standar -SANCO-)

Calibration graph (kurva kalibrasi): 2


konsentrasi boleh ( tidak boleh beda konsentrasi
lebih dari 10), Multi level kalibrasi lebih
disarankan -SANCO-

Addition Standar: penambahan standar


kedalam sampel
Metode Preparasi Standar
1.Standard in solvent
2.Matrix Match Calibration : Pembuatan standar
dalam matriks yang sama dengan matriks
sampel.
3.Matrix matched calibration with internal
standard : Penambahan standar internal.

Dalam Matrix matched calibration dibutuhkan


matriks yang tidak mengandung analit.

Matrix matched Calibration disarankan dalam


analisis MS berkaitan dengan Ionisation
Internal Standard
An internal standard (IS) is a chemical compound
added to the sample test portion or sample
extract in a known quantity at a specified stage
of the analysis, in order to check the correct
execution of (part of) the analytical method. The
IS should be chemically stable and/or typically
show the same behaviour as of the target
analyte.(SANCO)

Structural analogs of the analytes or isotopically


labeled internal standards (ILIS)
Clean Up QuEChERS
A clean-up, or dilution step may be necessary to
reduce matrix interferences and reduce
contamination of the instrument system leading
to an improved selectivity and robustness.
Concentration
Pemekatan/Penguapan
Concentration of sample extracts can cause
precipitation of matrix-components and in some
cases losses of pesticides.
To avoid losses during evaporation steps the
temperature should be kept as low as is
practicable.
A stream of dry nitrogen or vacuum centrifugal
evaporation is generally preferable to the use of
an air stream, as air is more likely to lead to
oxidation or the introduction of water and other
possible contaminants.
Sistem Deteksi
D2 ... the retention time of the analyte should
correspond to that of the calibration standard with
a tolerance of 0.2 min for both GC and LC
Reporting Result
The results from the individual analytes
measured must always be reported and their
concentrations expressed in mg/kg.
... residues of individual analytes below the RL
must be reported as < RL ...
Where a residue definition is expressed as a
sum of two or more measurable components,
the RL should be reported for each
measurable component separately ...
Where the residue definition includes more than
one analyte (Analit dan metabolitnya), the
respective sum of analytes must be
Interferences/Contaminant
Glassware that used in pesticide analysis must
be seperated for avoiding cross contamination.
Interferences by phthalate esters can pose a
major problem in pesticide determinations.
Interferences from phthalate esters can best be
minimized by avoiding contact with any
plastic materials.
Clean all glassware as soon as possible after
use by rinsing with the last solvent used.
This should be followed by detergent washing
with hot water, and rinses with tap water and
organic-free reagent water. Drain the
Validation
Linearity
Minimum 5 Levels, Criteria : Residual < +/- 20%
Specificity
Criteria : <30% of Residual Limit/LOQ
Matrix Effect
Accuracy & Precision
Acuracy/Trueness Criteria : Recovery = 70-120%
Precision criteria : RSD < 20%
Validation Planning

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