SAMPLE PREPARATION

Three key issues that often arise that necessitate pre-treatment of a

sample prior to analysis

• the sample is in the wrong physical state for the analysis method (e.g., the method
requires a liquid but you have a solid sample),
• the sample has interfering matrix components that may give either a false positive
or negative reading in the measurement,
• the sample has too low an analyte concentration to be detected by the
instrument.
 Solvent Extraction Method

• Solvent extraction is a method to separate compounds due to their unequal solubility in

two immiscible liquid phases, usually water and an organic solvent.
• The method is used to concentrate highly hydrophobic compounds, and consequently
increase analytical sensitivity.
• A buffer solution is added to sample to optimize the pH and target substance is then
extracted by an organic solvent such as ether and chloroform.
 PROBLEMS
A RnD Staff want to determine paracetamol (PCT) content on a liquid dosage form.
PCT standard were prepared in 1000ppm in ethanol. 100 microlitre of this solution was
take and put in a 5 mL volumetric flask, measure using spectrophotometer UV Vis and
have 0.231; 0.242; 0.239 as an absorbance after three times measurement. The
samples were prepared by dissolving 5 mL of PCT syrup in 10mL ethanol, filtered it
and add until 25mL of volumetric flask. sample solution then measured using
spectrophotometer UV Vis and have an absorbance 0.229; 0.234; 0.233 after three
times measurement. Calculate the percentage of PCT content in a sample.
 Problems
A QC staff have to determined vitamin C content in a cream. A Vitamin C standard was dissolved in an ethanol with a
different concentration and measured using UV Vis Spectrophotometry. The results depicted below:

No Concentration (ppm) Absorbance (average

after 3 measurement)
1 3 0.143
2 6 0,452
3 9 0,792
4 12 1,142
5 15 1,464

25 mg of cream sample was dissolved in 25 mL of ethanol then filtered, the filtrate were moved to a 50 mL of
volumetric flask and add until mark. 10microlitre of the solution was taken and put in 5 mL volumetric flask, ethanol
was added until mark. That solution was measured using UV spectrophotometer and got absorbance 0,511; 0,522;
0,513 after three measurement. Calculate vitamin C in that sample (%)