A new type of analytical morphological food device

The stock solution was prepared and weighed about 50.0mg Sudan red pigment standard. Sudan red and Sudan red peony were dissolved in acetonitrile. Sudan red ó and Sudan red were dissolved in chloroform, then the volume was adjusted to 50mL, and the working reserve was 1.0mg/mL. Store the stock solution in the dark and dilute to the desired concentration with acetonitrile.

LC/DAD-ESI/MS-MS analysis<5>Since the Sudan red series pigment is an azo compound, the abundance of negative ions is smaller and the sensitivity is less than the positive ionization mode; they are in ESI(+)-MS/MS conditions. The main ion ions formed by the cleavage of a hydroxyl group, an azo group and a carbon-nitrogen bond are as shown. Sudan red forms molecular ion peak of m/z249 +, mainly fragmented into m/z93, 156 and 232 daughter ions, of which the response of 232 is the largest, as the quantitative ion of Sudan red; Sudan red sputum forms the molecular ion peak of m/z277, fragmentation forms m/z120, The daughter ions of 156 and 260, with the m/z 260 daughter ion as the quantitative analysis ion of Sudan red peony; the molecular ion peak of Sudan red ó is m/z 353, mainly fragmented into 197 and 336, with m/z197 as quantitative analysis Ion; the molecular ion peak of Sudan red is m/z 381, which is mainly dissociated into m/z 209, 224, 276 and 364, and m/z 224 is used as a quantitative analysis ion. The Sudan Red series of pigments have a similar structure, so they have the same fragment ion peaks such as m/z 156, so the fragment ion peak should not be used as a quantitative analysis ion. Ion fragmentation of Sudan Red series pigment mass spectrometry.

The linear range is taken from the standard stock solution and diluted with acetonitrile to a standard working solution with a final mass concentration of 1.00 Lg/mL. The 10LL sample is taken and separated according to the above chromatographic separation conditions and mass spectrometry conditions. The experimental results show that the peak area (Y) and the concentration (X) of each substance in the Sudan Red series pigments are in a linear concentration range of 0.051.00 Lg/mL.

Recovery and precision test According to the above method, the blank sample (excluding Sudan Red series pigment) was subjected to spiked recovery test (addition amount 1.00Lg), pre-treatment according to the above sample processing method, repeated measurement 6 times, calculation of sample The spiked recovery rate. The average recovery rate of the four Sudan red pigments is between 86% and 98%.

Actual sample analysis As shown, a is a quantitative ion chromatogram obtained using a segmentation technique, with peaks 1, 2, 3, and 4 being Sudan red, ò, and ó, respectively. b Quantitative analysis of ion chromatograms of 剁 pepper-flavored radish samples submitted by a company. It can be seen from the figure that the sample contains Sudan red, which is confirmed by its bipolar mass spectrometry.

Conclusion HPLC-ESI/MS has an incomparable advantage for the simultaneous detection of Sudan Red series pigments in foods. It detects the concentration of a compound by detecting one or several representative m/z by selective ion channel. For some compounds with different m/z, even in the case of incomplete separation, selective ion channels It also removes the effects of interference peaks and achieves reliable results. This method has been applied to the confirmation of foods that may contain Sudan Red by the national standard method, and the effect is good.

The results of this study show that HPLC-ESI/MS has high selectivity, strong anti-interference ability, no false positive results, short analysis time, simple sample processing steps, etc. compared with the national standard high performance liquid chromatography. Advantages, therefore, it is recommended to add HPLC-MS method as a confirmation in the national standard method, and to confirm it by HPLC-MS when it is detected by HPLC-UV/Vis.

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