高效液相色谱法测定水产品中4-己基间苯二酚
详细信息Determination of 4-hexylresorcinol in aquatic products by high performance liquid chromatography
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摘要: 建立了水产品中4-己基间苯二酚（4-HR）残留量测定的高效液相色谱-荧光法。样品经乙腈提取,浓缩后用流动相溶解残渣,正己烷脱脂净化,过滤后供高效液相色谱（HPLC）分析。色谱条件为:WondaSilC18柱（250mm×4.6mm,5μm）;以甲醇-水（75:25,v/v）作为流动相,流速为1.0mL/min;荧光检测器激发波长为280nm,发射波长为310nm,外标法定量。结果表明:该方法在0.05～5.0μg/mL范围内线性关系良好,相关系数R2=0.9998。样品在0.1、0.2、1.0、5.0mg/kg加标水平时,平均回收率为90.9%～108.4%,相对标准偏差（RSD）为0.8%～8.1%（n=5）。方法定量限（LOQ）为0.1mg/kg。Abstract: A method for the determination of 4-hexylresorcinol in aquatic products was established by high performance liquid chromatography with fluorescence detection.The sample was extracted with acetonitrile and then the solvent extraction was evaporated to dryness.The residue was dissolved with the mobile phase followed by a clean-up step using n-hexane.The diluted solution was determined by HPLC.Chromatographic separation was carried out on a C18 column (250mm×4.6mm, 5μm) with elution of methanol-water solution (75:25, v/v) at a flow rate of 1.0mL/min.The fluorescence detection was performed at an excitation wavelength of 280nm and an emission wavelength of 310nm.4-hexylresorcinol was quantified by the external standard method.The calibration curves showed good linearity in the concentrations range of 0.05 ~ 5.0μg/mL for the standard solutions.The correlation coefficents (R2) was 0.9998.The average recoveries were 90.9% ~ 108.4% at spiked levels of 0.1, 0.2, 1.0 and 5.0 mg/kg.The relative standard deviations (RSD, n=5) were 0.8% ~ 8.1%.The limit of quantification (LOQ) was 0.1mg/kg.
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Keywords:
- HPLC;4-hexylresorcinol;aquatic products; /
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[1] 乔庆林.水产品褐变的原因和防止[J].海洋渔业, 1981, 2:23. [2] 姚兴存.虾类在冷冻加工中的褐变机理及其防止[J].冷藏技术, 1997, 81 (4) :27-29. [3] 郑丹, 段青源, 钟惠英, 等.甲壳类酪氨酸酶促褐变的研究进展[J].水产科学, 2008, 27 (8) :421-426. [4] 薛秀恒, 孟质文, 王志耕, 等.不同酶处理对冷藏鱼肉的新鲜度与褐变的影响[J].食品工业科技, 2011, 32 (4) :330-332. [5] 张艳, 王圣开.鱼肉蛋白质冷冻变性及抗冻剂的研究进展[J].肉类研究, 2008, 118 (12) :11-14. [6] McEvily A J, Iyengar R, Otwell S.Sulfite alternative prevents shrimp melanosis[J].Food Technol, 1991, 45 (9) :80-86.
[7] Frankos V H, Schmitt D F, Haws L C, et al.Generally recognized as safe (GRAS) evaluation of4-hyxylresorcinol for use as a processing aid for prevention of melanosis in shrimp[J].Regul Toxicol Pharmacol, 1991, 14 (2) :202-212.
[8] 凌关庭.4-己基间苯二酚 (4HR) :一种能抑制褐变的新型抗氧护色剂[J].食品工业, 1997, 3:19-20. [9] 食品安全国家标准.GB2760-2011食品添加剂使用标准[S].2011. [10] Joint FAO-WHO Expert Committee on Food Additives.Compendium of food additive specifications[M].Rome:FAO/WHO Press, 1995, 3:87-89.
[11] Montero P, Martinez-Alvarez O, Zamorano J P, et al.Melanosis inhibition and4-hexylresorcinol residual levels in deepwater pink shrimp (Parapenaeus longirostris) following various treatments[J].Eur Food Res Technol, 2006, 223 (1) :16-21.
[12] King J M, McEvily A J, Iyengar R.Liquid chromatographic determination of the processing aid4-hexylresorcinol in shrimp[J].Assoc Off Anal Chem, 1991, 74 (6) :1003-1005.
[13] Smallwood A W, Ranieri T L, Satzger R D.Determination of4-hexylresorcinol in crab meat[J].AOAC Int, 1998, 81 (2) :488-491.
[14] Jonker K M, Dekker C P.Determination of4-hexylresorcinol in shrimp by liquid chromatography with fluorescence detection[J].AOAC Int, 2000, 83 (1) :241-244.
[15] Nakazato M, Matsumoto H, Kasuya Y, et al.Determination of4-hexylresorcinol residues in prawn and crab[J].Food Hygienics Society of Japan, 2005, 46 (6) :282-285.
[16] Mendes R, Pestana J, Pestana C.Changes in4-hexylresorcinol residues during processing of deepwater pink shrimp (Parapenaeus longirostris) [J].Eur Food Res Technol, 2006, 223 (4) :509-515.
[17] 段小娟, 蔡发, 牟志春, 等.高效液相色谱荧光检测法测定虾中的4-己基间苯二酚[J].食品科学, 2009, 30 (14) :238-239. [18] 孙凯峰, 周陶忆, 顾蓓丽.虾中4-己基间苯二酚的检测技术研究[J].现代食品科技, 2010, 26 (3) :326-330. [19] 刘书成.水产食品加工学[M].郑州:郑州大学出版社, 2011:55.
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