全麦粉和小麦粉中烷基间苯二酚同系物组成的对比分析

doi:10.3864/j.issn.0578-1752.2020.10.012

Abstract

Abstract:

【Objective】 In order to realize the authenticity discrimination of whole wheat flour, a high performance liquid chromatography (HPLC) detection and analysis method was established to explore the composition of alkylresorcinols (ARs) homologues in whole wheat flour and refined wheat flour. 【Method】 The HPLC conditions were investigated to determine five kinds of ARs homologues, including 5-heptadecylresorcinol (C17:0), 5-nonadecylresorcinol (C19:0), 5-heneicosylresorcino (C21:0), 5-tricosylresorcinol (C23:0) and 5-hentacosylresorcinol (C25:0), and then a methodological evaluation was processed. The contents and composition of ARs homologues in 47 samples, including whole wheat flour, refined wheat flour and wheat bran from home and abroad, were determined and conducted by heat map and principal component analysis (PCA).【Result】 The chromatographic column of ZORBAX SB-C18 (150 mm×4.6 mm, 5 μm, Agilent ) was used for gradient elution, and the column was eluted with 0.1% formic acid aqueous solution and 0.1% formic acid methanol solution. The ARs homologues could be effectively separated within 35 minutes under the UV detection wavelength at 280 nm. The column temperature was 35℃, and the flow rate was 0.5 mL·min^-1with 20 μL injection. The peak shape of each homologue was symmetrical without interference, and the detected resolution was exactly. After methodological evaluation, the method was proved that it had good precision and sensitivity, the linear correlation coefficients of the standard curves were more than 0.999, the detection limit was 0.06-0.19 μg·mL ^-1, the recovery rate was 81.16%-112.92%, and the precision standard deviation was 0.02%-4.02%. Therefore, this method could be applied to determine the composition of ARs homologues. The composition of ARs homologues and total amount of ARs in different samples were found significantly after thermal cluster analysis (P<0.05). Among the ARs homologues of wheat flour samples, C21:0 was the highest, which accounted for 33%-61%; followed by C19:0, which accounted for 12%-44%; while the ratio of C17:0, C23:0 and C25:0 were the least. The content and abundance of ARs homologues in the whole wheat flour of United States and Canada were similar. The content of ARs homologues in abroad whole wheat flour was higher than the whole wheat flour in domestic. The composition of ARs homologues in domestic whole wheat flour was more abundant than refined wheat flour, except for individual refined wheat flour samples. The composition of homologous and total content of ARs in wheat bran F₁ were significantly higher than whole wheat flour and refined wheat flour (P<0.05). The total content of ARs in wheat bran F₁ was 1 795.78 μg·g^-1, which was the most significantly difference compared with other samples (P<0.05). The results of PCA showed that the main difference index between wheat flour samples was the composition of ARs homologues. As the first principal component, the cumulative contribution rate was 98.40%. The relative dispersion between wheat bran and other wheat flour samples was the farthest, while the dispersion of Chinese refined wheat flour was the largest. Even the whole wheat flour of United States and Canada could nearly overlapped, the whole wheat flour and part of refined wheat flour of China could only partially overlapped.【Conclusion】 The HPLC method could be employed to effectively and rapidly quantify the ARs in whole wheat flour products. Moreover, the abundance of ARs homologues in whole wheat flour was better than that of ARs homologues in refined wheat flour under comparative analysis. In summary, the results could provide a theoretical basis for authenticity discrimination and quality control for whole wheat flour by exploring the composition of ARs homologues.

Key words: wheat, whole wheat flour, alkylresorcinols, high performance liquid chromatography, homologues, authenticity discrimination

ZOU YanYu,FANG Yong,LI Peng,HUANG QinQin,XIA Ji,LIU Qin,XIE MinHao,HU QiuHui. Comparative Analysis of Alkylresorcinols Homologue Composition in Whole Wheat Flour and Refined Wheat Flour[J].Scientia Agricultura Sinica, 2020, 53(10): 2055-2065.

Figures/Tables 5

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烷基间苯二酚ARs	线性方程 Linear equation	相关系数 Correlation coefficient (R²)	线性范围 Linearity range (μg?mL^-1)	检出限 LOD (μg?mL^-1)	定量限 LOQ (μg?mL^-1)	相对标准偏差 RSD (%)
C17:0	y=6.344x-1.060	0.9998	1—50	0.06	0.20	3.69
C19:0	y=1.701x-7.916	0.9991	5—500	0.18	0.61	0.98
C21:0	y=4.176x-10.02	0.9995	5—500	0.18	0.59	1.19
C23:0	y=3.836x-3.391	0.9997	1—200	0.19	0.63	2.90
C25:0	y=1.917x+0.418	0.9995	2—100	0.18	0.61	4.89

小麦粉 Wheat flour	加标浓度 Added value (μg?mL^-1)	回收率测定值 Recovery value (%)			平均值±标准偏差 Mean±SD (%)	相对标准偏差 RSD (%)
小麦粉 Wheat flour	加标浓度 Added value (μg?mL^-1)	1	2	3	平均值±标准偏差 Mean±SD (%)	相对标准偏差 RSD (%)
C17:0	1	81.53	80.35	83.87	81.92 ± 1.79	2.18
	10	85.37	84.90	85.84	85.37 ± 0.47	0.55
	50	81.89	80.44	81.13	81.16 ± 0.73	0.89
C19:0	5	109.44	108.85	110.62	109.60 ± 0.90	0.82
	100	87.25	87.25	87.55	87.35 ± 0.17	0.19
	500	84.13	83.17	83.22	83.51 ± 0.54	0.64
C21:0	5	87.69	92.72	94.88	91.76 ± 3.69	4.02
	100	91.10	91.77	91.98	91.62 ± 0.46	0.50
	500	84.37	84.36	84.45	84.39 ± 0.05	0.05
C23:0	1	113.09	112.05	113.61	112.92 ± 0.80	0.71
	20	101.91	100.34	101.12	101.12 ± 0.78	0.77
	100	85.50	85.48	85.48	85.49 ± 0.02	0.02
C25:0	5	87.45	81.19	83.17	83.94 ±3.20	3.81
	20	98.81	92.28	93.12	94.74 ±3.55	3.75
	100	98.32	93.05	94.98	95.45 ±2.67	2.79

Comparative Analysis of Alkylresorcinols Homologue Composition in Whole Wheat Flour and Refined Wheat Flour

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