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以4-fluoro-3-nitrobenzo-trifluoride(FNBT)为衍生剂,N,N-diisopropylethyl-amine(DIPEA)为催化剂,建立了一种新的柱前衍生-反高效液相色谱检测法(RP-HPLC)同时测定酱腌菜中的8种生物胺(组胺、色胺、β-苯乙胺、腐胺、酪胺、尸胺、亚精胺及精胺)。采用硼酸盐缓冲溶液为衍生介质,在60℃下衍生反应30 min,使用C18色谱柱分离,以乙腈和超纯水为流动相梯度洗脱,流速1.00m L/min,紫外检测波长242 nm。在0.5~100 mg/L浓度范围内,8种生物胺呈现良好的线性相关(r2≥0.999),方法的检出限(LODs)为0.013~0.053 mg/L,定量限(LOQs)为0.044~0.176 mg/L,加标平均回收率为93.47%~99.87%,相对标准偏差(RSD)为0.47%~3.67%。采用该方法对26种市售酱腌菜中的生物胺进行了分析,发酵型酱腌菜中的生物胺总量范围为40.57~692.82 mg/kg,非发酵型酱腌菜中的生物胺总量范围为9.86~270.93 mg/kg。发酵型酱腌菜中8种生物胺单体的平均含量均高于非发酵型酱腌菜。该方法简单、准确和可靠,可适用于酱腌菜中生物胺的快速分析。
A new pre-column derivatization-reverse-phase high performance liquid chromatography (RP-HPLC) method was developed using 4-fluoro-3-nitrobenzo-trifluoride (FNBT) as a derivatizing agent and N, N-diisopropylethyl-amine HPLC) Simultaneous determination of eight biogenic amines (histamine, tryptamine, beta-phenylethylamine, putrescine, tyramine, cadaverine, spermidine and spermine) in pickles. Using borate buffer solution as the derivatization medium, the reaction was carried out at 60 ℃ for 30 min, separated on a C18 column and eluted with acetonitrile and ultrapure water as the mobile phase at a flow rate of 1.00 mL / min. The UV detection wavelength was 242 nm . There were good linear correlations (r2 ≥0.999) for the eight biogenic amines in the range of 0.5-100 mg / L, the limits of detection (LODs) were 0.013-0.053 mg / L and the LOQs were 0.044 ~ 0.176 mg / L. The average recoveries of spiked samples ranged from 93.47% to 99.87% and the relative standard deviations (RSDs) ranged from 0.47% to 3.67%. The biogenic amines in 26 kinds of commercial pickles were analyzed by this method. The total amount of biogenic amines in the fermented pickles ranged from 40.57 to 692.82 mg / kg. The biogenic amines in the non-fermented pickles The amount range of 9.86 ~ 270.93 mg / kg. The average content of eight biogenic amines in fermented pickles was higher than that in non-fermented pickles. The method is simple, accurate and reliable and can be applied to the rapid analysis of biogenic amines in pickles.