Komponen Kualitas Data Hasil Analisis

4 1 : Kualifikasi instrumen = Membuktikan kelayakan

instrumen

3 2 : Validasi Metode Analisis = Membuktikan

kelayakan prosedur analisis

2 3: Sistem Suitability Test = Verifikasi performa

sistem analisis memenuhi kriteria kelayakan

1 4: QC Check = Verifikasi akurasi analisis sampel

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 Analisis Pestisida dalam buah apel (Agilent Method)

Metode Quantitasi dalam MS

1. External Calibration: Satu konsentrasi standar ( C sample +/- 30% dari standar -SANCO-)
2. Calibration graph (kurva kalibrasi): 2 konsentrasi boleh ( tidak boleh beda konsentrasi lebih dari
10), Multi level kalibrasi lebih disarankan -SANCO-
3. Addition Standar: penambahan standar kedalam sampel

Minimal dalam satu batch analisis dilakukan kalibrasi standar.

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 Surpression.

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.

Recovery Check During Analysis

Generalised acceptance criteria : 60-140% at concentration correspond to sample, or at RL and 2-

10x RL

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 calculated.
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 glassware and dry it in an oven at 130 OC for several
hours, or rinse with methanol and drain. Store dry glassware in a clean environment.

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