UHPLC-MS/MS Determination of 4-Hexylresorcinol in Shrimps with Solid Phase Extraction
摘 要
采用固相萃取-超高效液相色谱-串联质谱法测定虾类中4-己基间苯二酚的含量。样品的匀浆(5.00 g)用甲醇提取两次(每次10 mL),合并提取液。移取提取液5 mL,并用水定容至10 mL。此溶液通过PRIME HLB固相萃取柱净化,用含1%(质量分数)氨水的甲醇-乙腈(9+1)溶液4 mL洗脱,洗脱液于40℃水浴中氮气吹至近干,残留物用乙腈(6+4)溶液1 mL溶解。以Waters Acquity UPLC BEH C18色谱柱为分离柱,以不同体积比的水和乙腈的混合液为流动相进行梯度洗脱,采用电喷雾负离子源和多反应监测模式检测。4-己基间苯二酚的质量浓度在1.0~100.0 μg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.25 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为70.1%~88.6%,测定值的相对标准偏差(n=6)为3.8%~6.4%。
Abstract
UHPLC-MS/MS was applied to the determination of 4-hexylresorcinol in shrimps with solid phase extraction. Homogenized pulp (5.00 g) of the sample was extracted twice with methanol (10 mL each). 5 mL of the combined extract was taken,and then made up to 10 mL with water. The solution was purified by passing through PRIME HLB SPE column,and then eluted with 4 mL of mixture of methanol and acetonitrile (9+1) containing 1% (mass fraction) ammonia. The eluate was evaporated to near dryness by N2-blowing at 40℃ in the water bath.The residue was taken up with 1 mL of acetonitrile (6+4) solution. Waters Acquity UPLC BEH C18 chromatographic column was used as stationary phase, and the mixture of acetonitrile and water mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Linear relationship between values of peak area and mass concentration of 4-hexylresorcinol was kept in the range of 1.0-100.0 μg·L-1, with detection limit (3S/N) of 0.25 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method. Values of recovery found were in the range of 70.1%-88.6%, with RSD's (n=6) in the range of 3.8%-6.4%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201805025
所属栏目 专题报道(食品分析)
基金项目 水产品质量安全风险监测能力建设项目(2016F10024)
收稿日期 2017/9/20
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备注高学慧,硕士研究生,主要从事水产品加工与贮藏研究工作
引用该论文: GAO Xuehui,HAO Yunbin,ZHANG Xiaojun,MEI Guangming,CHEN Si,YAN Zhongyong. UHPLC-MS/MS Determination of 4-Hexylresorcinol in Shrimps with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(5): 606~610
高学慧,郝云彬,张小军,梅光明,陈思,严忠雍. 固相萃取-超高效液相色谱-串联质谱法测定虾类中4-己基间苯二酚[J]. 理化检验-化学分册, 2018, 54(5): 606~610
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参考文献
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【2】俞所银,李越华,任青,等.虾类保鲜研究进展[J].食品工业科技, 2013,34(6):396-400.
【3】李馥君,翁佩芳,朱亚珠,等.中国毛虾(Acetes chinensis)虾皮复合保鲜剂筛选及保鲜效果的研究[J].食品工业科技, 2017,38(6):333-338.
【4】钱韻芳,谢晶,吴文惠.虾类保藏过程中酚氧化酶酶促黑变作用机理及其抑制方法的研究进展[J].食品工业科技, 2012,33(22):400-405.
【5】MCEVILY A J, IYENGAR R, OTWELL S. Sulfite alternative prevents shrimp melanosis[J]. Food Technology, 1991,45(9):80-86.
【6】FRANHOS V H, SCHMITT D F, HAWS L C, et al. Generally recognized as safe (GRAS) evalution of 4-hexylresorcinol for use as a processing aid for prevention of melonosis in shrimp[J]. Regulatory Toxicology Pharmacology, 1991,14(2):202-212.
【7】KING J M, MCEVILY A J, IYENGAR R. Liquid chromatographic determination of the processing aid 4-hexylresorcinol in shrimp[J]. Journal-Association of Official Analytical Chemists, 1991,74(6):1003-1005.
【8】周会玲,魏敏,唐爱君,等.4-己基间苯二酚对鲜切苹果褐变及品质的影响[J].食品研究与开发, 2013,34(8):100-103.
【9】王毓.超高效液相色谱-串联质谱法测定鲜切杏鲍菇中4-己基间苯二酚的含量[J].分析试验室, 2015,34(8):954-957.
【10】邱丰艳,丁力,陈雪梅.超高效液相色谱-串联四极杆质谱法测定鸡腿菇中4-己基间苯二酚的含量[J].理化检验-化学分册, 2016,52(5):514-517.
【11】MONTERO P, MARTINEZ-ÁLVAREZ O, ZAMORANO J P, et al. Melanosis inhibition and 4-hexylresorcinol residual levels in deepwater pink shrimp (Parapenaeus longirostris) following various treatments[J]. European Food Research & Technology, 2015,223(1):16-21.
【12】DAI X Y, ZHANG M X, WEI X Y, et al. Novel multifunctional hydroxypyridinone derivatives as potential shrimp preservatives[J]. Food & Bioprocess Technology, 2016,9(7):1079-1088.
【13】余颖.气相色谱-质谱法测定甲壳类水产品中4-己基间苯二酚残留[J].福建水产, 2015,37(3):227-232.
【14】高平,黄国方,黄和,等.高效液相色谱法测定水产品中4-己基间苯二酚[J].食品工业科技, 2013,34(1):304-308.
【15】唐利平,邓启华,谢家理.UPLC-MS/MS法测定虾蟹中4-己基间苯二酚的残留量[J].中国测试, 2015,41(7):60-63.
【16】严忠雍,张小军,李奇富,等.免疫亲和柱净化-液相色谱-串联质谱法测定海洋生物中河豚毒素[J].分析化学, 2015,43(2):277-281.
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