Introduction

FAREVA is one of worldwide leaders of outsourcing in the Industrial & Household, Cosmetics and Pharmaceutical fields. They propose different services to their clients: research, formulation, manufacturing and filling. Their principal aim is to meet the clients ‘specifications and so assure quality products. To develop a method of cleaning validation it is then important to avoid the contaminations during the formulation step. FCA and Farevabio, 2 sites decided to work together on this project. Isopropyl Myristate is very used in the formulation of cosmetic and pharmaceutical products. Hence it is used as a tracer to check the good cleaning of Farevabio vats. To start, we defined LOD and LOQ of the method.

Experimental conditions

A calibration with 3 points was necessary. First the standard solution, was prepared with 5.0 g of palmitate isopropyl and 96 % volume ethanol until 100 mL. Then, 3 standards with 2 mL of standard solution were realized with different concentrations: 5 000 PPM, 500 PPM and 50 PPM. The rinsing waters were injected directly and twice. The blank was done with ethanol. Finally, the order of injections was: blank, standard 1, standard 2, standard 3, blank and 2 injections of rinsing waters. Results were imported in an excel file and the unknown concentrations were calculated automatically. We had to have a coefficient R² more than 0.999.

Results

To check the LOQ, we calculated S/N of standard 3: S/N = (2xH) / h. H was the height of the peak and h the height of the background noise. S/N had to be higher than 10. For this method and analytic conditions, the S/N of standard 1 was more than 10. Then: LOQ = 50 PPM and LOD= 16.67 PPM.

Conclusion

Three interpretations are possible in function of the results. If it is more than 16.67 PPM Isopropyl Myristate is “not detectable”, it is between 16.67 PPM and 50 PPM the compound is detectable but “not quantifiable” and if it is more than 50 PPM it is necessary to carry out another concentration standard.

Table 1: Table of parameters and conditions of GC.

Figure 1: Temperature program Figure 2 : Chromatogram of standard 3 solution

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SECRETARY
Catherine BEKHALED