Page 93 - Application Notebook - Solution for Food Safety

Application No. AD-0096 N
News

Spiked Milk Samples and Recovery
A blank milk sample and two spiked samples of 13
mixed standards in the same blank were obtained from
an analytical laboratory, labeled as Blank, S1 (spiked
100 μg/L) and S2 (spiked 1,000 μg/L). The blank milk
matrix was analyzed first and the result showed no any
detection of the 13 bisphenols studied.
The chromatogram of spiked sample S1 is shown in
Fig. 5. The quantitative results and recovery data of the
13 bisphenols in both samples are tabulated in Table 3.
In both samples, the measured concentrations of
BADGE-H 2O-HCI are higher than the expected levels
with a recovery around 130 %. On the other hand, three
compounds with longer retentions (peaks 11 to 13)
exhibit much lower concentrations as expected and
low recovery of about 40 % and 60 %.

UHPLC-RF Chromatogram of Spiked Milk Sample S1
(100 μg/L). The Sample was Diluted with Water for Two Time
Prior to Injection (10 μL)

Table 3 Analysis Results of Spiked Milk Samples for 13 Bisphenols Determined by the UHPLC-RF Method Established
Spiked S1 Spiked S2
ID # Name Ret Time (min)
Conc. (μg/L) Recovery % Conc. (μg/L) Recovery %
1 BFDGE-2H2O 7.9 115.0 115 1140.8 114.1
2 BADGE-2H2O 9.5 114.5 114.5 1123.6 112.4
3 BPF 13.4 114.9 114.9 1152.4 115.2
4 BPA 18.1 114.1 114.1 1162.9 116.3
5 BADGE-H2O-HCL 19.4 131.3 131.3 1284.9 128.5
6 BADGE-H2O 19.9 91.1 91.1 983.1 98.3
7 BFDGE-2HCL-1 26.9 79.3 79.3 947.6 94.8
8 BFDGE-2HCL-2 27.8 90.5 90.5 983.0 98.3
9 BFDGE-1 28.9 68.6 68.6 823.8 82.4
10 BFDGE-2 30.0 77.2 77.2 824.2 82.4
11 BADGE-2HCL 31.8 47.3 47.3 668.9 66.9
12 BADGE-HCL 33.0 43.3 43.3 635.7 63.6
13 BADGE 34.3 37.4 37.4 563.7 56.4

 Conclusions
An UHPLC method with using a high sensitivity <References>
1
fluorescence detector was developed for fast, well- * : Jan Poustka, Lenka Dunovs ká, Jana Hajšlová, Kateřina Holadová
separation and high sensitivity analysis of thirteen and Ivana Poustková, Czech J. Food Sci., Vol. 25, No. 4: 221–229
(2007)
bisphenols, including the most concerned BPA, BPF, * : vana Poustkov, Jaroslav DobiD, Ingrid Steiner, Jan Poustka, Michal
2
BADGE and BFDGE, in milk samples. Voldrˇich, Eur Food Res Technol (2004) 219:534–539.
3
This new method shows high sensitivity to low μg/L * : United States Food and Drug Administration web site: Bisphenol
levels, high accuracy and excellent repeatability. The A (BPA) for Use in Food Contact Applications 4. Application News
No. L408, Shimadzu Corporation.
method was applied to spiked milk samples and the
results indicated the good feasibility, high sensitivity
and reliability in simultaneous determination of
thirteen bisphenols in milk samples.

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