PKKK/300/UP/061 Identification & Determination of p-phenylenediamine in Hair Care Products
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NPRA PUSAT KAWALAN KUALITI |
ARAHAN KERJA: IDENTIFICATION & DETERMINATION OF P-PHENYLENEDIAMINE IN HAIR CARE PRODUCTS | |
| No. Dokumen: PKKK/300/UP/061 | Terbitan / Semakan: Terbitan 3 Semakan 0 | |
| Tarikh Kuatkuasa: 10 April 2026 | Bahagian / Unit: SPPK · Unit Penyaringan | |
0.0 SEJARAH PINDAAN & SEMAKAN
Sejarah Pindaan & Semakan Dokumen (18 entri) ▸
Terbitan 1 Semakan 1:
Pinda para 1.0 Objective
Tambah para 6.1 Test Method for Identification
Tambah para 6.2 Test Method for Quantitation
Tukar susunan nombor para 6.3, 6.4, 6.5 & 6.6
Terbitan 1 Semakan 2:
Pinda tajuk dokumen dari Determination of p- Phenylenediamine in Hair Care Products
(Penentuan p- Phenylenediamine dalam Produk Penjagaan Rambut) kepada Identification & Determination of p- Phenylenediamine in Hair Care Products
(Identifikasi & Penentuan p- Phenylenediamine dalam Produk Penjagaan Rambut)
Terbitan 2 Semakan 0 :
Pinda no dokumen dari PKKK/300/KOS/033 kepada PKKK/300/UP/061.
Pinda tarikh kuatkuasa 3 Februari 2026 kepada 10 April 2026.
Kemaskini para 7.0 Quality Records :
KOS/X004 kepada UP/X010
KOS/X006 to UP/X011
KOS/X003 kepada UP/X009
KOS/002A kepada UP/002B
KOS/X009 kepada UP/X013
1.0 OBJECTIVE
The test is performed to identify the presence of p-phenylenediamine and quantify the amount present in hair care products using HPLC.
2.0 SCOPE
This method describes the determination of p-Phenylenediamine in hair care products.
Head of Section
Head of Unit
Distribute samples for testing to Pharmacist through QUEST system
Validate and approve analysis result on QUEST system
Review investigation report of failed samples
Pharmacist
Distribute samples for testing among analysts
Ensure tests are conducted according to laboratory protocols
Review analysis reports and enter results into the QUEST system
Investigate and report failed samples
Pharmacy Assistants (Analysts)
Perform sample testing according to the approved procedure
Prepare test reports
Equipment/ Materials
Ultrapure water
Acetonitrile, HPLC grade
Potassium Dihydrogen Phosphate, KH2PO4
Disodium Hydrogen Phosphate, Na2HPO4
1-Heptanesulfonic Acid, Sodium Salt
Sodium Ascorbate
Phosphate Buffer (25 mM/L phosphate buffer-0.1% heptane sulphonic acid): Dissolve by shaking 3.06 g KH2PO4, 0.38 g Na2HPO4 and 1 g sodium salt of 1-heptane sulfonic acid in 1 L water. Fill up to the mark and mix. Adjust to pH 6.0 by the addition of sodium hydroxide (NaOH) or phosphoric acid (H3PO4)
0.5% Sodium Ascorbate Solution: Dissolve 1.25 g sodium ascorbate in 250 mL of phosphate buffer.
Diluent: Mixture of 0.5% sodium ascorbate solution and Acetonitrile (ACN) in 4:6 ratio
Reference standard: p-Phenylenediamine
Volumetric Flasks (amber), Class A
Ultrasonicator Bath
PTFE Membrane Syringe Filter 0.45µm
HPLC Parameters
6.0 PROCEDURE
Note: The preparation can be modified as long as the final concentration is achieved.
System Suitability
Tailing factor should be NMT 2.0
Theoretical plates should be NLT 1500
Test Method for Quantitation
Standard Stock Preparation 0.8 mg/mL (freshly prepared)
Note: The preparation can be modified as long as the final concentration is achieved.
Sequence of Injection
System Suitability Test (SST)
Relative Standard Deviation (RSD) of retention time NMT 2.0 %
Tailing factor should be NMT 2.0
Theoretical plates should be NLT 1500
Sample Preparation
Make up to the mark with diluent and mix well.
Heat the solution in water bath at around 60 ± 1 ºC for about 5 minutes.
Perform the HPLC determination within 24 hours after preparation of the samples.
Note: Due to the nature of sample (easily oxidised), sample weight and dilution factor may be adjusted depending on concentration of p-Phenylenediamine in the sample. Concentration of sample should fall within the standard calibration range.
Sample Spike Preparation (IQC)
Result Interpretation:
Compare the retention time and spectrum obtained from the sample chromatogram with that of p-Phenylenediamine standard solution chromatogram.
The identity of p-Phenylenediamine is positive if the retention time and the UV spectrum of sample is similar to that obtained from the standard solution.
Calculations
Plot a calibration curve and determine the amount of p-Phenylenediamine in %w/w.
7.0 QUALITY RECORDS
Borang Tatacara Pengujian menggunakan kaedah HPLC : UP/X010
Borang Pengiraan Ujian Kuantifikasi Teknik Kromatografi : UP/X011
Rumusan Laporan Pengujian Kromatografi : UP/X009
Laporan Siasatan Sampel Tidak Lulus Ujian Kromatografi : UP/002B
Borang Keputusan Ujian Kosmetik : UP/X013
8.0 ATTACHMENTS
NA
Jadual Kromatografi & Rujukan Data
| Terbitan | Semakan | Ditulis Oleh | Disemak Oleh | Diluluskan Oleh | Tarikh Kuatkuasa |
|---|---|---|---|---|---|
| 1 | 0 | Gopinatha Ganesh | Leong Lip Wai | Nor Izyani Hanafi | 1 Ogos 2024 |
| 1 | 1 | Gopinatha Ganesh | Nur Syazana Ahmad Nordin | Nor Izyani Hanafi | 26 Disember 2025 |
| 1 | 2 | Gopinatha Ganesh | Nur Syazana Ahmad Nordin | Nor Izyani Hanafi | 3 Februari 2026 |
| 2 | 0 | Gopinatha Ganesh | Tan Lu Yi | Ida Syazrina Ibrahim | 10 April 2026 |
| RUJUKAN | RUJUKAN |
|---|---|
| No. Dokumen | Tajuk |
| 15th ACTLC – ACM PPD Singapore |
| Column | : | Discovery® RP Amide C16, 25cm x 4.6mm, 5µm or equivalent |
|---|---|---|
| Run Time | : | 30 minutes (Isocratic) |
| Mobile phase | : | Phosphate Buffer : Acetonitrile 90:10% v/v Note: Mobile phase mixture ratio may be adjusted depending on the sample matrix |
| Column Oven | : | 25 ºC |
| Flow rate | : | 1.0 mL/min |
| Detection | : | UV, 235 nm and 295 nm |
| Injection volume | : | 10 µL |
| Sequence of Injection | Injection ID | Run time (min) |
|---|---|---|
| 1 | Blank/ diluent | 30 |
| 2 | SST (Std A) – 1x | 30 |
| 3 | Blank/ diluent | 30 |
| 4 - 8 | Sample solution | 30 |
| 9 | Blank/ diluent | 30 |
| Std A (LOQ) [0.024 mg/mL] | Transfer by pipette 3 mL stock solution in a 10 mL volumetric flask, fill up to the mark with diluent and mix. Further dilute by pipetting another 2 mL of the solution to a 20-mL volumetric. Fill up to the mark with diluent and mix. |
|---|---|
| Std B [0.24 mg/mL] | Transfer by pipette 3 mL stock solution in a 10 mL volumetric flask, fill up to the mark with diluent and mix. |
| Std C [0.32 mg/mL] | Transfer by pipette 4 mL stock solution in a 10 mL volumetric flask, fill up to the mark with diluent and mix. |
| Std D [0.4 mg/mL] | Transfer by pipette 5 mL stock solution in a 10 mL volumetric flask, fill up to the mark with diluent and mix. |
| Std E [ 0.48 mg/mL] | Transfer by pipette 6 mL stock solution in a 10 mL volumetric flask, fill up to the mark with diluent and mix. |
| Std F [ 0.56 mg/mL] | Transfer by pipette 7 mL stock solution in a 10 mL volumetric flask, fill up to the mark with diluent and mix. |
| Sequence of Injection | Injection ID | Run time (min) |
|---|---|---|
| 1 | Blank/ diluent | 30 |
| 2 | SST (Std C) – 6x | 180 |
| 3 | IQC Solution | 30 |
| 4 - 9 | Std A - F | 180 |
| 10 | IQC Solution | 30 |
| 11 | Sample solution A | 30 |
| 12 | Sample solution B | 30 |
| 13 | IQC Solution | 30 |
| Content (%w/w) | = | Concentration in sample obtained from calibration curve (mg/mL) | x | Volume (mL) | x Dilution | x 1 | x | Purity | x | 100 |
|---|---|---|---|---|---|---|---|---|---|---|
| Content (%w/w) | Concentration in sample obtained from calibration curve (mg/mL) | Weight of sample (mg) | factor | 1000 | ||||||
| Content (%w/w) | Concentration in sample obtained from calibration curve (mg/mL) | Weight of sample (mg) |