Determination of Formaldehyde in Fruits and Vegetables by HPLC

doi:10.7506/spkx1002-6630-201622030

Abstract

Abstract: A high performance liquid chromatography (HPLC) method was used to determine formaldehyde in fruits and vegetables by formaldehyde derivation with pentafluorophenylhydrazine (PFPH). Samples were extracted and derived at 70 ℃ with ultrasonicaction for 30 min. After completion of the reaction, centrifugation was carried out and the supernatant was purified and analyzed by HPLC. The quantitation was performed using the external standard method. The separation was performed on an XDB-C18 column (4.6 mm × 250 mm, 5 μm) in an isocratic elution mode using a mobile phase consisting of acetonitrile and water (70:30, V/V) at a flow rate of 1.0 mL/min. The column temperature was 40 ℃ and detection wavelength was 258 nm. The results showed that the limit of quantification (LOQ) of the presented method was 0.114 mg/kg, with a good linear relationship in the range of 0.114–57 mg/L. The average recovery rates at three spiked levels were 81.4%–101.8%, with relative standard derivation (RSD) of 2.6%–5.0% (n = 6). The method was simple, stable and suitable for the determination of formaldehyde in fruits and vegetables with a low limit of detection (LOD).

Key words: fruits and vegetables, formaldehyde, HPLC, pentafluorophenylhydrazine

CLC Number:

TS255.7

LI Jun, LIU Yongxiang, WANG Hui, LIU Jia, LIU Hui, KAN Jianquan,*. Determination of Formaldehyde in Fruits and Vegetables by HPLC[J]. FOOD SCIENCE, 2016, 37(22): 198-204.

References

[1] TONG Z Q, HAN C S, MIAO J Y, et al. Excess endogenous formaldehyde induces memory decline[J]. Progress in Biochemistry and Biophysics, 2011, 38(6): 575-579. DOI:10.3724/SP.J.1206.2011.00241.
[2] SONGUR A, OZEN O A, SARSILMAZ M. The toxic effects of formaldehyde on the nervous system[J]. Reviews of Environmental Contamination and Toxicology, 2010, 203: 105-118. DOI:10.1007/978-1-4419-1352-4_3.
[3] ANDERSEN M E, CLEWELL H J, BERMUDEZ E, et a1. Formaldehyde: integrating dosimetry, cytotoxicity, and genomics to understand dose-dependent transitions for an endogenous compound[J]. Toxicological Sciences, 2010, 118(2): 716-731. DOI:10.1093/toxsci/kfq303.
[4] LI W W, GUO H, FAN G W, et al. Advance in study on endogenous formaldehyde and pathogenesis of Alzheimer’s disease[J]. China Journal of Chinese Materia Medica, 2012, 37(20): 3071-3020. DOI:10.4268/cjcmm20122004.
[5] 俞其林, 励建荣. 食品中甲醛的来源与控制[J]. 现代食品科技, 2007(10): 55-59. DOI:10.3969/j.issn.1673-9078.2007.10.024.
[6] 励建荣, 朱军莉. 食品中内源性甲醛的研究进展[J]. 中国食品学报, 2011, 11(9): 247-256. DOI:10.3969/j.issn.1009-7848.2011.09.027.
[7] LIU Y, YE Z, YANG H, et al. Disturbances of soluble N-ethylmaleimide-sensitive factor attachment proteins in hippocampal synaptosomes contribute to cognitive impairment after repetitive formaldehyde inhalation in male rats[J]. Neuroscience, 2010, 169(3): 1248-1254. DOI:10.1016/j.neuroscience.2010.05.061.
[8] 周福林, 宋少飞, 张稳婵, 等. 催化动力学光度法测定腐竹中的痕量甲醛[J]. 食品科学, 2009, 30(10): 191-193. DOI:10.3321/j.issn:1002-6630.2009.10.042.
[9] ZHU J L, LI J R, JIA J. Effects of thermal processing and various chemical substances on formaldehyde and dimethylamine formation in squid Dasidicas gigas[J]. Journal of the Science of Food and Agriculture, 2012, 92(12): 2436-2442. DOI:10.1002/jsfa.5649.
[10] 杜永芳, 柳淑芳, 马敬军, 等. 测定水产品中甲醛含量的分光光度法研究[J]. 中国食品学报, 2005, 5(3): 91-96. DOI:10.3969/j.issn.1009-7848.2005.03.017.
[11] LI J R, ZHU J L, YE L F. Determination of formaldehyde in squid by highperformance liquid chromatography[J]. Asia Pacific Clinical Nutrition, 2007, 16(1): 127-130. DOI:10.6133/apjcn.2007.16.s1.24.
[12] ZHU Y, PENG Z Q, WANG M, et al. Optimization of extraction procedure for formaldehyde assay in smoked meat products[J]. Journal of Food Composition and Analysis, 2012, 28(1): 1-7. DOI:10.1016/j.jfca.2012.07.002.
[13] 杨娟, 秦樱瑞, 曾艺涛, 等. 内源性甲醛、甲醛毒性及甲醛抑制物的研究进展[J]. 食品科学, 2014, 35(1): 294-297. DOI:10.7506/spkx1002-6630-201401058.
[14] WENG X, CHON C H, JIANG H, et al. Rapid detection of formaldehyde concentration in food on a polydimethylsiloxane (PDMS) microfluidic chip[J]. Food Chemistry, 2009, 114(3): 1079-1082. DOI:10.1016/j.foodchem.2008.10.027.
[15] 王小波, 李国强, 孟建新, 等. 甲基橙-溴酸钾体系催化光度法测定微量甲醛[J]. 分析科学学报, 2004, 20(3): 335-336. DOI:10.3969/j.issn.1006-6144.2004.03.035.
[16] WANG T, GAO X L, TONG J, et al. Determination of formaldehyde in beer based on cloud point extraction using 2,4-dinitrophenylhydrazine as derivative reagent[J]. Food Chemistry, 2012, 131(4): 1577-1582. DOI:10.1016/j.foodchem.2011.10.021.
[17] BIANCHI F, CARERI M, MUSCI M, et al. Fish and food safety: Determination of formaldehyde in 12 fish species by SPME extraction and GC-MS analysis[J]. Food Chemistry, 2007, 100(3): 1049-1053. DOI:10.1016/j.foodchem.2005.09.089.
[18] 芮露明, 彭增起, 汪敏, 等. GC-MS法测定烟熏腊肉中的甲醛含量[J]. 食品科学, 2014, 35(8): 142-146. DOI:10.7506/spkx1002-6630-201408028.
[19] 王术皓, 牛学丽, 杜凌云, 等. 溴酸钾氧化中性红动力学光度法测定甲醛[J]. 分析科学学报, 2004, 20(2): 215-216. DOI:10.3969/j.issn.1006-6144.2004.02.031.
[20] LI Z W, MA H B, LU H H, et al. Determination of formaldehyde in foodstuffs by flow injection spectrophotometry using phloroglucinol as chromogenic agent[J]. Talanta, 2008, 74(4): 788-792. DOI:10.1016/j.talanta.2007.07.011.
[21] 邵仕萍, 相大鹏, 李华斌, 等. 乙酰丙酮衍生化高效液相色谱-荧光检测法测定食品中的甲醛[J]. 食品科学, 2015, 36(16): 241-245. DOI:10.7506/spkx1002-6630-201516046.
[22] WANG H, DING J, DU X B, et al. Determination of formaldehyde in fruit juice based on magnetic strong cation-exchange resin modified with 2,4-dinitrophenylhydrazine[J]. Food Chemistry, 2012, 131(1): 380-385. DOI:10.1016/j.foodchem.2011.08.056.
[23] XU X, SU R, ZHAO X, et al. Determination of formaldehyde in beverages using microwave-assisted derivatization and ionic liquidbased dispersive liquid-liquid microextraction followed by highperformance liquid chromatography[J]. Talanta, 2011, 85(5): 2632-2638. DOI:10.1016/j.talanta.2011.08.037.
[24] REBECCA A, TRENHOLM, FEMANDO L. Analysis of formaldehyde formation in wastewater using on-fiber derivatization-solid-phase microextraction-gas chromatography-mass spectrometry[J]. Journal of Chromatography A, 2008, 25(29): 26-29. DOI:10.1016/j.chroma.2008.09.044.
[25] 尤铁学. 碘量法标定二氧化硫和甲醛标准贮备溶液的改进[J]. 化学试剂, 2008, 30(6): 447-448. DOI:10.3969/j.issn.0258-3283.2008.06.016.