PRE-TREATMENT OF COSMETICS SAMPLES.Here’s an overview based on the provided search results.

Pre-treatment of cosmetic samples is a crucial step in the analytical process, primarily aimed at ensuring accurate and reliable results when analyzing the complex matrices found in cosmetic products. Here’s an overview based on the provided search results.

1. PRE-TREATMENT OF COSMETICS SAMPLES.

2. Contents. Introduction Cosmetics Types of Extractions Analysis

3. Introduction What is mean by pre-treatment of samples ? 3 Sample pre-treatment is critical for identification, confirmation and quantification of samples. It is necessary to convert the samples into form of suitable for the measurement & step must also be performed without loss of any unplanned modification of secondary samples. It also require to provide representative , reproducible & homogeneous solution for ; ICP NMR tube MS AAS GC/LC

4. Cosmetics Decoratives Nail polish Cocealer Foundations Skin-care Moisturizers Sunscreens Cleanser Hair-care Shapoo Conditioners Wax & gels Perfumes Parfum Eau -de-parfum Eau -de- toilett 4 What is mean by cosmetics ? Cosmetics are constituted mixtures of chemical compounds derived from naturally or synthetically created ones , intended to the human body by being rubbed, poured to clean, improve or change the complexion, skin, hair, nails or teeth. Types of cosmetics :

5. Pre-treatment of solid samples ; Solid-phase extraction Supercritical fluid extraction Pressurized liquid extraction Pre-treatment of liquid samples ; Liquid-liquid extraction Solid-supported liquid extraction Solid-phase Micro-Extraction Types of pre-treatment of samples by state :-

6. Pre-Treatment of Solid Samples I. Solid-Phase Extraction :- Principle :- In Solid –Phase Extraction the solid particulates uses to serve as adsorbent material. SPE is a separation process by which compounds that are dissolved or suspended in a liquid mixture are separated from other compounds in a mixture according to their physical & chemical properties Types of Device Format :- Cartridge SPE Pipette

7. 7 Conditioning :- conditioned” by solvent methanol (MeOH) or acetonitrile (ACN). Sample Loading :- sample dissolved in a weak solvent & that allows strong retention of the analyte Washing :- It involves removal of interferences by washing (rinsing) the cartridge with a solvent of intermediate strength. Elution :- Supply of eluting solvent that removes analyte from adsorbent material.  

8. 8 Matrix Sample Amount. Sample Pretreatment. Eluting Solvent Analysis. Anti-acne samples, Creams, lotions, Shampoos, Lipsticks, Sunscreens 0.5 g (water soluble products), 0.1-0.25 g (water insoluble products) Dilution in 10 mL MeOH/H2O centrifugation, evaporation, reconstitution with 2 mL MeOH/H2O 4 mL MeOH/H2O LC/GC/MS /UV 85-90 % ( Recovery ) Solid – Phase Extraction for Cosmetic Samples :-

9. 9 II. Supercritical fluid extraction :- Principle :- A  supercritical fluid  (CO2) originates from a fluid being forced to pressure and temperature that is above its critical point causing the liquid and gas phases to become indistinguishable from each other.    CO2 + Polar organic solvents Enhance dissolution ability. Polar Solvets :- Methonol , Acetonitrile etc.

10. 10 Matrix Sample Amount Sample Pre-Treatment Eluting Solvent Analysis Moisturizers, shampoos, lotions, soaps, antiperspirants, sunscreens, 0.5 g – 1.0 g of sample SF CO2 +Dilution in 10 mL ACN/H2O (2% formic acid ) reconstitution with 2 mL H2O (0.1% formic acid) 1 mL (×2) MeOH: HPLC/GC/MS 80-85% ( RECOVERY ) Supercritical Fluid Extraction for Cosmetic :-

11. 11 III. Pressurized Fluid Extraction : Principle :- Pressurized fluid extraction (PFE) is an automated extraction technique that uses elevated temperature (50-200 °C) and pressure (150-2000 psi) to increase the rate and efficiency of the extraction process.  Pressurized fluids, such as subcritical water, pressurized aqueous ethanol and pressurized aqueous ionic liquids Samples are placed in the cell body along with an inert granular matrix. Solvent is pumped into the cell until it is filled, and then allowed to equilibrate under static conditions. After a predetermined time, the extract is pumped out of the cell and is collected for analysis.

12. 12 Matrix Sample Amount Sample Pre-Treatment Eluting Solvent Analysis Moisturizing creams, lotions, sunscreens, hair productsnail polishes 0.1g – 1.0 g (Water Souble ) 1.0 – 4.0 g ( Water Insolubles ) Mixture with 2 g Na2SO4 + 2 g Florisil 10 mL ACN GCMS/MS 80-85 % Recovery Pressurized Fluid Extraction of Samples :-

13. 13 Principle :- Liquid-liquid extraction (LLE) is useful for separating analytes from interferences by partitioning the sample between two immiscible liquids or phases. Aqueous phase the aqueous phase often can be injected directly onto a reversed-phase HPLC column. An organic solvent. Analytes extracted into the organic phase are easily recovered by evaporation of the solvent. The most popular approach to LLE uses a separatory funnel . I. Liquid Liquid Extraction :- Pre-Treatment Of Liquid Samples :-

14. 14 Analytes Matrix Sample Amount Sample Pre-Treatment Eluting Solvent Analysis 4 phenols Cosmetics 0.1 g – 0.5 g Organic Solvent mixed with sample. EtOH/H2O (1:1) LC-MS 6 plasticizers, 7 preservatives Shower Gels 0.1 g – 0.5 g Organic Solvent mixed with sample. 5 mL MeOH UHPLC-MS Liquid-Liquid Extraction method of Sample Pre-Treatment :-

15. 15 II. Supported/Solid Liquid Extraction :- Principle :- Solid-liquid extraction is a type of extraction process of extraction which is performed between the solid and liquid phases. In this type of extraction solute particle (dispersed phase) is in a solid state and the solvent(dispersed medium) is in the liquid state.Solid -liquid extraction is a method that is used mainly to remove soluble components from solids using a solvent. Step-1 Step-2 Step-3

16. 16 Analytes Matrix Sample Amount Sample Pre-Treatment Eluting Solvent Analysis 8 preservatives, 14 dyes Lipsticks, lotions, creams, masks, shampoos, gels, soaps, gels, toothpastes 0.1 g – 1.0 g Mixture with 100 mg C18 1.5 mL MeOH LC-MS/MS 2 preservatives, 2 phthalates Perfumes, shampoos, creams, body milks, shower gels ,Hair dyes 0.5 g – 1.0 g Dilution in 10 mL H2O. 10 mL EtOH (perfumes), 10 mL H2O + 10 mL MTBE GC-MS Solid-Liquid Extraction method of Sample Pre-Treatment :-

17. 17 III Solid – Phase Micro Extraction :- Principle :- SPME relies on the extraction of solutes from a aqueous sample into an absorptive polymeric layer coated onto a solid fused silica fiber the extraction reaches equilibrium. Then the SPME fiber and captured solutes are transferred into an inlet system that then desorbs the solutes into a gas (for GC) or liquid (for LC) mobile phase.

18. 18 Extraction :- An externally coated SPME absorptive layer, the layer is exposed to sample in the liquid phase or gas phase (headspace) Transfer :- Transfer the SPME layer and absorbed analytes away from sample to exposure for desorption in chromatography mobile phase. Desorption :- Absorbed solutes to desorb with as close to 100%

19. 19 Solid Phase Microextraction for Cosmetic :- Analytes Matrix Sample Amount Sample Pre-treatment Eluting Solvent Analysis 16 preservatives Sunscreen, lotions, creams, s, hair conditioners 0.1 g – 1.0 g & 1 ml – 2 ml Dilution in 10 mL H2O + 20% NaCL + derivatization - GC-MS/MS BHT Cosmetics 0.1 g – 1.0 g Dilution in 4 mL H2O, centrifugation - GC-MS

20. 20 Referances :- Snyder, L.R.; Kirkland, J.J.; Dolan, J.W. Introduction to Modern Liquid Chromatography, 3rd Ed., Chapter 2 and Appendix I.2, John Wiley and Sons, Hoboken. Gledhill, S. High Sensitivity Detection of Pesticides in Water Using On-line SPE Enrichment, Agilent Technologies Application Note. Sample Pre Treatment Fundamentals of Chromatography. https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8399500/ https://www.sciencedirect.com/topics/earth-and-planetary-sciences/sample-preparation.

21. Thank you.