Rapid Determination of Residual Amount of Benzo(a)pyrene in Fruit-Vegetable Chips by High Performance Liquid Chromatography
摘 要
建立了高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量的方法。样品经正己烷提取,苯并(a)芘分子印迹柱净化后,经Eclipse Plus C18色谱柱(150 mm×4.6 mm,5.0 μm)分离,以体积分数为90%的乙腈溶液为流动相进行等度洗脱。结果表明:苯并(a)芘的质量浓度与其对应的峰面积在0.4~100 μg·L-1内呈线性关系,相关系数为0.999 9。测定下限(10S/N)为0.40 μg·kg-1。以果蔬脆片样品为基质在3个浓度水平下进行加标回收试验,所得日内回收率为89.4%~93.7%,测定值的相对标准偏差(n=6)为4.3%~7.2%;日间回收率为87.6%~92.5%,测定值的相对标准偏差(n=6)为5.8%~8.4%。用此方法分析了20个果蔬脆片样品,在7个样品中检出了苯并(a)芘,但其含量均小于GB 2762-2017规定的限量(10 μg·kg-1)。
Abstract
A method for the rapid determination of residual amount of benzo(a)pyrene residues in fruit-vegetable chips with high performance liquid chromatography was developed. The fruit-vegetable chip sample was extracted with n-hexane, and then purified with benzo(a)pyrene molecularly imprinted column. The sample solution obtained was separated with a Eclipse Plus C18 chromatographic column (150 mm×4.6 mm, 5.0 μm), and eluted isocratically with using acetonitrile solution with volume fraction of 90% as mobile phase. Results were found that the linearity relationship between mass concentration of benzo(a)pyrene and its respective peak area was kept in the range of 0.4-100 μg·L-1, with correlation coefficient of 0.999 9. Lower limit of determination (10S/N) found was 0.40 μg·kg-1. The spiked recovery was made at 3 concentration levels by using fruit-vegetable chip samples as matrix, giving recoveries (n=6) of inter-day and intra-day in the ranges of 89.4%-93.7% and 87.6%-92.5%, with RSDs (n=6) of determined values of inter-day and intra-day in the ranges of 4.3%-7.2% and 5.8%-8.4%, respectively. The prescribed method was used in analyzing the 20 fruit-vegetable chip samples, and benzo(a)pyrene was found in 7 samples, with content all lower than limit (10 μg·kg-1) specified by GB 2762-2017.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202101007
所属栏目 工作简报
基金项目 出入境检验检疫行业标准制修订计划项目(2015B187K);潍坊市科学技术发展计划(2015ZJ1101)
收稿日期 2020/1/15
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备注郭礼强,高级工程师,硕士,主要从事食品中有毒有害残留检测方面的研究,glq1980@sina.com
引用该论文: GUO Liqiang,DING Kuiying,ZHANG Jinling,ZHANG Yan. Rapid Determination of Residual Amount of Benzo(a)pyrene in Fruit-Vegetable Chips by High Performance Liquid Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(1): 36~40
郭礼强,丁葵英,张金玲,张艳. 高效液相色谱法快速测定果蔬脆片中苯并(a)芘残留量[J]. 理化检验-化学分册, 2021, 57(1): 36~40
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【3】周娜,骆和东,李耀群.食品中苯并(a)芘的微波辅助萃取方法的研究[J].光谱学与光谱分析, 2014,34(3):787-790.
【4】MO R, ZHANG Y, NI Z, et al. Determination of benzo[a]pyrene in camellia oil via vortex-assisted extraction using the UPLC-FLD method[J]. Food Science and Biotechnology, 2017,26(1):15-19.
【5】GAZIOGLU I, TEKKELI S E K. Development and validation of a HPLC method for the determination of benzo(a)pyrene in human breast milk[J]. Food Science and Biotechnology, 2017,26(2):319-322.
【6】GUO Y, ZHAO W J, DENG Z F, et al. Determination of benzo[α]pyrene in edible oil using tetraoxocalix
【7】arene
【8】triazine bonded silica SPE sorbent[J]. Food Additives & Contaminants Risk Assess, 2018,35(7):1356-1365.
【9】LUO K, GAO Q, HU J. Determination of 3-hydroxybenzo[a]pyrene glucuronide/sulfate conjugates in human urine and their association with 8-hydroxydeoxyguanosine[J]. Chemical Research in Toxicology, 2019,32(7):1367-1373.
【10】WU M L, CHEN T Y, CHEN W J, et al. Carbon fiber ionization mass spectrometry coupled with solid phase microextraction for analysis of benzo[a]pyrene[J]. Analytical Chimica Acta, 2019,1049:133-140.
【11】何旭东,李红梅.高效液相色谱-荧光法测定食用油中苯并芘含量[J].安徽农学通报, 2018,24(9):135-136.
【12】任道援,骆书娜,卢叶,等.高效液相色谱-荧光法快速测定茶籽油中苯并(a)芘的残留[J].广州化工, 2018,46(14):88-90.
【13】郝媛媛.高效液相色谱法测定野山茶油中苯并芘的含量[J].理化检验-化学分册, 2018,54(7):816-818.
【14】黄坤,王幸平,尹佳,等.高效液相色谱法测定大米和小麦粉中的苯并(α)芘[J].粮食与油脂, 2018,31(10):86-88.
【15】梁瑞,段兰萍,黄瑞,等.固相萃取-高效液相色谱法测定粮油中苯并芘残留[J].粮食科技与经济, 2016,41(5):46-49.
【16】YANG S D, TANG T, TAN Y M, et al. Determination of benzo(a)pyrene in fried and baked foods by HPLC combined with vesicular coacervative supramolecular solvent extraction[J]. Journal of Food Science and Technology, 2019,56(1):428-435.
【17】王浩,刘艳琴,杨红梅,等.高效液相色谱法测定化妆品中苯并芘残留[J].分析试验室, 2010,29:221-222.
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