Application of isotope dilution-liquid chromatography-tandem mass spectrometry in the preparation and certification of reference material of tenuazonic acid and tentoxin in wheat flour

doi:10.3724/SP.J.1123.2019.12005

Abstract

Abstract:

A method for the preparation and certification of the reference material of tenuazonic acid (TeA) and tentoxin (TEN) in wheat flour was developed. This method provided methodological references to develop of standard material for analyzing alternaria toxins in grains. The wheat flour reference materials were based on wheat grains which were naturally contaminated with alternaria toxins. The certified values for TeA and TEN were determined by isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) and cooperated certification of multiple laboratories. The wheat flour reference materials were stored at room temperature, protected from light and characterized by low uncertainty. The wheat flour reference materials are currently the only wheat flour reference materials that naturally contaminate TeA and TEN, and it can be used in the evaluating related analytical methods involved in food safety risk monitoring, product quality testing and quality control measurements.

Key words: liquid chromatography-tandem mass spectrometry (LC-MS/MS), reference material, tenuazonic acid (TeA), tentoxin (TEN), alternaria toxins, wheat flour

XIE Ji'an, LIU Bolin, ZHAO Ziwei, ZHANG Lei, YANG Dajin, ZHAO Yunfeng. Application of isotope dilution-liquid chromatography-tandem mass spectrometry in the preparation and certification of reference material of tenuazonic acid and tentoxin in wheat flour[J]. Chinese Journal of Chromatography, 2020, 38(7): 833-840.

Figures/Tables 11

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Compound	Parent ion (m/z)	Product ions (m/z)	Cone voltage/V	Collision energies/eV
* Quantitative ion.
TeA	196.0	139.1^*, 112.1	52	20, 24
¹³C₂-TeA	198.1	141.1	52	20
TEN	413.2	141.1^*, 271.1	50	22, 18
D₃-TEN	416.4	141.1	50	22

Compound	Parent ion (m/z)	Product ions (m/z)	Cone voltage/V	Collision energies/eV
* Quantitative ion.
TeA	196.0	139.1^*, 112.1	52	20, 24
¹³C₂-TeA	198.1	141.1	52	20
TEN	413.2	141.1^*, 271.1	50	22, 18
D₃-TEN	416.4	141.1	50	22

Compound	Blank/ (μg/kg)	Added/ (μg/kg)	Detected/(μg/kg)
Compound	Blank/ (μg/kg)	Added/ (μg/kg)	Matrix standard curve method	Isotope internal standard dilution method
TeA	＜0.5	10	9.68	10.04
	＜0.5	50	48.8	50.2
	＜0.5	200	197.5	200.6
TEN	＜0.1	2.0	1.93	2.01
	＜0.1	10	9.73	10.07
	＜0.1	40	38.9	40.2

Compound	Blank/ (μg/kg)	Added/ (μg/kg)	Detected/(μg/kg)
Compound	Blank/ (μg/kg)	Added/ (μg/kg)	Matrix standard curve method	Isotope internal standard dilution method
TeA	＜0.5	10	9.68	10.04
	＜0.5	50	48.8	50.2
	＜0.5	200	197.5	200.6
TEN	＜0.1	2.0	1.93	2.01
	＜0.1	10	9.73	10.07
	＜0.1	40	38.9	40.2

Compound	Added/ (μg/kg)	Content/ (μg/kg)	Recovery/ %	RSD/ %
TeA	10	9.89	98.9	3.8
	50	51.72	103.4	2.4
	200	209.12	104.6	1.5
TEN	2.0	1.99	99.6	3.1
	10	10.08	100.8	2.2
	40	41.47	103.7	1.4