腌干鱼制品中8种生物胺测定方法的优化
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陈玉峰(1989-),男,硕士研究生,研究方向为水产品质量安全,hsxycyf1989920@163.com

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国家自然科学基金项目(31371800);中国水产科学研究院基本科研业务费(2014C05XK01);广东省海洋渔业科技推广专项(A201301C01, A201201I04)


Optimizing the analyzing method for determining 
8 biogenic amines in salted-dried fish
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    摘要:

     建立了反相HPLC同时测定色胺、2-苯乙胺、腐胺、尸胺、组胺、酪胺、亚精胺和精胺8种生物胺的方法,并对腌干鱼制品中生物胺的提取方法进行了优化。1,7-二氨基庚烷为内标,经丹磺酰氯衍生,C18柱(250 mm × 4.6 mm,5 μm)分离后,使用荧光检测器检测,荧光激发波长为350 nm,发射波长为520 nm;乙腈-乙酸铵-超纯水为流动相进行梯度洗脱,流速为1 mL/min;采用NaOH及饱和NaHCO3调节衍生体系pH,三氯乙酸(TCA)、高氯酸(HClO4)和盐酸(HCl)作为提取介质对腌干鱼制品中生物胺进行提取。结果显示,8种生物胺在30 min 内完全分离,并呈良好的线性相关性(R2 ≥ 0.998 66);精胺的线性范围为0.5~50.0 μg/mL,其余7种生物胺为0.5~100.0 μg/mL;最低检测限为0.03~0.10 μg/mL;仪器精密度较好(RSD≤1.87%);最佳衍生体系pH为11.0;5% TCA提取生物胺效果最为理想;腌干鱼样品中8种生物胺得到有效检测结果,生物胺总量范围为(91.75±3.11)~(986.43±5.42) mg/kg。该方法适合腌干鱼制品等腌制水产品中8种常见生物胺的快速有效检测。[中国渔业质量与标准,2014,4(4):41-48]

    Abstract:

     A reversed-phase high performance liquid chromatographic (HPLC) method was established to determine tryptamine, 2-phenylethylamine, putrescine, cadaverive, histamine, tyramine, spermidine and spermine in salted-dried fish and the extraction method of biogenic amines was optimized. Biogenic amines in salted-dried fish were derived with dansyl chloride. 1,7-Diaminoheptane was used as an internal standard(IS). 8 biogenic amines were separated by C18 column(250 mm×4.6 mm, 5 μm), and then detected by fluorescence detector with excitation wavelength of 350 nm and emission wavelength of 520 nm. Gradient elute using a mobile phase composed of acetonitrile, ammonium acetate and ultrapure water was at 1 mL/min flow rate. Sodium hydroxide and saturated sodium bicarbonate were used to adjust pH of derivative system and biogenic amines were extracted with trichloroacetic acid (TCA) or perchloric acid (HClO4) or hydrochloric acid (HCl). The results indicated that 8 biogenic amines completely separated within 30 min, and the correlation coefficient (R2) was greater than 0.998 66; linear range of spermine was among 0.5~50.0 μg/mL; linear range of the other biogenic amines were among 0.5~100.0 μg/mL. The limits of detection were in the range of 0.03~0.10 μg/mL. The relative standard deviation (RSD) of precision was lower than 1.87%. The pH 11.0 was most suitable for derivative system. The using of 5% TCA for extracting biogenic amines in salted-dried fish was a more suitable extraction than the others. Biogenic amines in seven salted-dried fish were determined effectively and the values of total biogenic amines were in the range of (91.75±3.11)~(986.43±5.42) mg/kg. So this optimized method is a rapid, efficient detection way for 8 biogenic amines in salted-dried aquatic product. [Chinese Fishery Quality and Standards, 2014, 4(4):41-48]

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陈玉峰,吴燕燕*,等.腌干鱼制品中8种生物胺测定方法的优化[J].中国渔业质量与标准,2014,4(4):41-48. CHEN Yufeng, WU Yanyan*,et al.

Optimizing the analyzing method for determining 
8 biogenic amines in salted-dried fish
[J]. Chinese Fishery Quality and Standards,2014,4(4):41-48.

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  • 最后修改日期:2014-10-11
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