Page 15 - Shimadzu Journal vol.7 Issue2

Food Development

vapor pressure, which was in agreement with the report by Bimakr et Garlic samples were spiked with mixed phenolic compound standards
[11]
al . On the other hand, the increase in temperature could also induce at 0.8 µg/g, 1 µg/g and 2 µg/g, which were used to assess the accuracy
faster molecular desorption and diffusion and contribute to the extraction and precision of this method. The recoveries at the 3 spiked concentrations
efficiency. In summary, the optimization results indicated that extracting were 63–131.5%, 71.8–109.5% and 64.1–110.4%, respectively. Except
the 15 phenolic compounds at 50ºC in 9 min with the addition of 30% ferulic acid and quercetin, which were spiked at the level of 0.8 µg/g,
methanol was the best set of off-line SFE conditions. In addition, the accuracies of most of the target analytes were acceptable for the
subcritical phase could be eventually reached for SFE with these general analytical method. Meanwhile, most RSD values for the evaluation
optimized factors, it is necessary to extract polar compounds in of precision (repeatability of the recovery) were lower than 10%.
samples, especially for phenolic compounds.
Real sample analysis
Method validation
Finally, our established method was used to measure 11 phenolic
Sample pretreatment of offline SFE is shown in Fig 2. The pretreatment compounds in garlic from the four main producing areas of China. The
process is rather simple. The developed off-line SFE-SFC-MS/MS method detection results indicate that ferulic acid was detected in all four
for phenolic compounds was validated. Each standard solution of the origins (Cangshan, Jinxiang, Pizhou, and Dali) at relatively high levels,
phenolic compounds with the concentrations of 5, 10, 20, 50, 100, from 0.47 to 0.86 µg/g, while different types of phenolic compounds
200, 500 and 1000 ng/mL was mixed with 0.5 g garlic and extracted were found in samples collected from the different locations. All of
by SFE. A total of 11 phenolic compounds was screened, presented these results suggest that this off-line SFE-SFC-MS/MS method could
acceptable linearity (R2> 0.99) over the concentration range of 0.02–8 µg/g. be adapted for the qualitative and quantitative analysis of the phenolic
The LODs of the 11 phenolic compounds varied from 0.6 to 12 ng/g, compounds in garlic.
and the scope of the LOQs ranged from 2 to 40 ng/g.

Fig. 2 Sample pretreatment of offline SFE

Conclusions quercetin and related flavonols, Food Chem. 77 (2002) 177–185.
[6] C.L. Silva, N. Haesenb, J.S. Câmara, A new and improved strategy
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SFE-SFC-MS/MS method has been developed for the analysis of with ultrahigh pressure liquid chromatography for analysis of lowmolecular
phenolic compounds in garlic. After the careful optimization of the weight polyphenols in vegetables, J. Chromatogr. A 1260 (2012)
SFE parameters, phenolic compounds were successfully extracted in 154–163.
less than 13 min. Besides, a matrix matched standard was employed [7] Y. Huang, T. Zhang, H. Zhou, Y. Feng, C. Fan, W. Chen, J. Crommen,
for removing matrix effects and phenolic compounds showed acceptable Z. Jiang, Fast separation of triterpenoid saponins using supercritical
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samples, animal samples and other food samples. extraction of vegetable matrices: Applications, trends and future
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