柱前衍生高效液相色谱法测定5种常见食用菌中的甲醛含量
|
摘要
目的建立柱前衍生-高效液相色谱法测定5种常见食用菌中甲醛含量。方法将干制与新鲜食用菌用超纯水浸泡,浸泡液经2,4-硝基苯肼(DNPH)衍生后,采用高效液相色谱法检测;色谱柱:C18(250mm×4.6mm,5μm),流动相:乙腈-水(70:30, V:V);流速为1.0 mL/min;检测波长352 nm;柱温40℃。外标法定量测定食用菌中甲醛含量。结果柱前衍生法对甲醛浓度在10.70～214.00μg/L范围内与其衍生物峰面积呈良好的线性关系,线性回归系数(r~2)为0.9964,方法的检出限为4.20μg/kg(S/N=3)。加标回收率为78.27%～114.26%,精密度1.55%～9.22%(n=6)。5种食用菌样品仅香菇样品检出甲醛。新鲜香菇甲醛含量超标,干制后香菇甲醛含量降低,低至国家标准含量以下。结论本研究的方法简便、快速、准确、稳定,可用于测定食用菌中甲醛含量。
Objective To establish a method for determination of formaldehyde content in 5 kinds of common edible fungi by pre-column derivatization-high performance liquid chromatography. Methods The dried and fresh edible fungus were soaked with ultra-pure water, the solution was derived from 2,4-nitrophenylhydrazine(DNPH)and detected by high performance liquid chromatography(HPLC). Chromatographic column was C18(250 mm×4.6 mm, 5 μm), mobile phase was 70% acetonitrile and 30% water, and flow rate was 1.0 mL/min. The detection wavelength was 352 nm. The column temperature was 40 ℃. The external standard method was used to quantitatively detect the formaldehyde in edible fungi. Results The calibration curve of the concentration of formaldehyde showed good linearity within 10.70-214.00 μg/L, with the linear regression coefficient(r~2) was 0.9964, and the limit of detection of the method was 4.20 μg/kg(S/N=3). The average recoveries were 78.27%-114.26%, and the relative standard deviations were 1.55%-9.22%(n=6). Formaldehyde was detected only in mushrooms. The formaldehyde content in fresh mushrooms was exceed, but the formaldehyde content in dried mushrooms was reduced and below the national standards. Conclusion This method is simple, rapid, accurate and stable, which can be used to determine the content of formaldehyde in edible fungi.
Objective To establish a method for determination of formaldehyde content in 5 kinds of common edible fungi by pre-column derivatization-high performance liquid chromatography. Methods The dried and fresh edible fungus were soaked with ultra-pure water, the solution was derived from 2,4-nitrophenylhydrazine(DNPH)and detected by high performance liquid chromatography(HPLC). Chromatographic column was C18(250 mm×4.6 mm, 5 μm), mobile phase was 70% acetonitrile and 30% water, and flow rate was 1.0 mL/min. The detection wavelength was 352 nm. The column temperature was 40 ℃. The external standard method was used to quantitatively detect the formaldehyde in edible fungi. Results The calibration curve of the concentration of formaldehyde showed good linearity within 10.70-214.00 μg/L, with the linear regression coefficient(r~2) was 0.9964, and the limit of detection of the method was 4.20 μg/kg(S/N=3). The average recoveries were 78.27%-114.26%, and the relative standard deviations were 1.55%-9.22%(n=6). Formaldehyde was detected only in mushrooms. The formaldehyde content in fresh mushrooms was exceed, but the formaldehyde content in dried mushrooms was reduced and below the national standards. Conclusion This method is simple, rapid, accurate and stable, which can be used to determine the content of formaldehyde in edible fungi.
引文
[1]吕玉琼,林凯,侯穗波,等.香菇中甲醛含量的监测报告[J].中国卫生检验杂志,2002,12(6):701.Lv YQ,Lin K,Hou SB,et al.Monitoring report of formaldehyde content in Lentinus edodes[J].Chin J Health Lab Technol,2002,12(6):701.
[2]彭锦峰,刘景富,邰超,等.HPLC法测定食用香菇中甲醛的含量[C].中国环境保护优秀论文集,2005.Peng JF,Liu JF,Tai C,et al.Determination of formaldehyde in edible Lentinus edodes by HPLC[C].Excellent Collection of Papers on Environmental Protection in China,2005.
[3]马敬军,周德庆,柳淑芳,等.二硝基苯肼衍生-高效液相色谱法测定水产品中甲醛含量的研究[J].海洋水产研究,2005,26(1):28-31.Ma JJ,Zhou DQ,Liu SF,et al.Determination of formaldehyde in aquatic products by HPLC with dinitrophenylhydrazine derivatization[J].Marine Fish Res,2005,26(1):28-31.
[4]宋凤英,王永芳,韩宏伟,等.食品中甲醛测定值的探讨[J].实验技术与方法,2002,14(3):20-23.Song FY,Wang YF,Han HW,et al.Discussion on determination value of formaldehyde in food[J].Exp Tech Methods,2002,14(3):20-23.
[5]王成云,龚叶青,谢堂堂,等.柱前衍生/高效液相色谱法测定皮革中甲醛含量[J].皮革科学与工程,2011,21(6):47-52.Wang CY,Gong YQ,Xie TT,et al.Determination of formaldehyde in leathers by pre-column derivation/ultra performance liquid chromatography method[J].Leather Sci Eng,2011,21(6):47-52.
[6]曹国华,郑剑萍,杜玮,等.柱前衍生高效液相色谱法测定盐酸四环素原料药中微量甲醛含量[J].中国药业,2015,(6):42-43:44.Cao GH,Zheng JP,Du W,et al.Determination of trace formaldehyde in tetracycline hydrochloride raw material medicine by precolumn derivatization HPLC[J].China Pharm,2015,(6):42-43:44.
[7]郭飞燕,于海霞,马轩,等.高效液相色谱法测定人造板中甲醛含量的新方法[J].林业工程学报,2015,29(6):109-112.Guo FY,Yu HX,Ma X,et al.Determination of formaldehyde in wood-based panels by high performance liquid chromatography[J].China Forest Sci Technol,2015,29(6):109-112.
[8]龙举,张小军,郭远明,等.高效液相色谱法测定海捕鱼中甲醛的含量[C].2013年浙江省渔业科技论坛论文集,2013.Long J,Zhang XJ,Guo YM,et al.Determination of formaldehyde in sea fish by high performance liquid chromatography[C].Collection of BBSPapers on Fishery Science and Technology of Zhejiang Province in 2013,2013.
[9]赵婷,赵梅,温正如,等.高效液相色谱法测定织物涂层整理剂中的甲醛含量[J].陕西科技大学学报(自然科学版),2009,27(2):69-72.Zhao T,Zhao M,Wen ZR,et al.Determination of formaldehyde content in textile coating agents by high performance liquid chromatography method[J].J Shaanxi Univ Sci Technol(Nat Sci Ed),2009,27(2):69-72.
[10]冯敏铃,李盛安.高效液相色谱法测定大白菜中甲醛残留效果研究[J].现代农业科技,2013,(9):281,284.Feng ML,Li SA.Determination of formaldehyde residue in Chinese cabbage by high performance liquid chromatography[J].Mod Agric Sci Technol,2013,(9):281,284.
[11]王圣庆,郭瑛,马言顺,等.柱前衍生高效液相色谱法测定啤酒中微量甲醛[J].化学研究与应用,2006,18(2):214-216.Wang SQ,Guo Y,Ma YS,et al.Determination of trace formaldehyde in beer by HPLC with precolumn derivatization and UV detection[J].Chem Res Appl,2006,18(2):214-216.
[12]甘凝岚,颜春荣,徐春祥,等.高效液相色谱法测定鸭血制品中甲醛含量[J].食品科学,2014,35(12):204-207.Gan NL,Yan CR,Xu CX,et al.Determination of formaldehyde in duck blood products by HPLC[J].Food Sci,2014,35(12):204-207.
[13]王帆,王勇,黄洁玉,等.纺织品中游离甲醛含量的高效液相色谱法测定[J].分析科学学报,2006,22(4):428-430.Wang F,Wang Y,Huang JY,et al.Determination of free formaldehyde in textiles by high performance liquid chromatography[J].J Anal Sci,2006,22(4):428-430.
[14]吴新华,朱瑞芝,陆舍铭,等.高效液相色谱法测定香精中甲醛的含量[J].化学试剂,2010,32(9):817-818,858.Wu XH,Zhu RZ,Lu SM,et al.Determination of formaldehyde in flavors using high performance liquid chromatography[J].Chem Reagent,2010,32(9):817-818,858.
[15]李向荣,黄亚羲.高效液相色谱法测定草酸二甲酯中甲醛含量[J].分析仪器,2013,(5):15-17.Li XR,Huang YX.Determination of formaldehyde in dimethyl oxalate by HPLC[J].Anal Instrum,2013,(5):15-17.
[2]彭锦峰,刘景富,邰超,等.HPLC法测定食用香菇中甲醛的含量[C].中国环境保护优秀论文集,2005.Peng JF,Liu JF,Tai C,et al.Determination of formaldehyde in edible Lentinus edodes by HPLC[C].Excellent Collection of Papers on Environmental Protection in China,2005.
[3]马敬军,周德庆,柳淑芳,等.二硝基苯肼衍生-高效液相色谱法测定水产品中甲醛含量的研究[J].海洋水产研究,2005,26(1):28-31.Ma JJ,Zhou DQ,Liu SF,et al.Determination of formaldehyde in aquatic products by HPLC with dinitrophenylhydrazine derivatization[J].Marine Fish Res,2005,26(1):28-31.
[4]宋凤英,王永芳,韩宏伟,等.食品中甲醛测定值的探讨[J].实验技术与方法,2002,14(3):20-23.Song FY,Wang YF,Han HW,et al.Discussion on determination value of formaldehyde in food[J].Exp Tech Methods,2002,14(3):20-23.
[5]王成云,龚叶青,谢堂堂,等.柱前衍生/高效液相色谱法测定皮革中甲醛含量[J].皮革科学与工程,2011,21(6):47-52.Wang CY,Gong YQ,Xie TT,et al.Determination of formaldehyde in leathers by pre-column derivation/ultra performance liquid chromatography method[J].Leather Sci Eng,2011,21(6):47-52.
[6]曹国华,郑剑萍,杜玮,等.柱前衍生高效液相色谱法测定盐酸四环素原料药中微量甲醛含量[J].中国药业,2015,(6):42-43:44.Cao GH,Zheng JP,Du W,et al.Determination of trace formaldehyde in tetracycline hydrochloride raw material medicine by precolumn derivatization HPLC[J].China Pharm,2015,(6):42-43:44.
[7]郭飞燕,于海霞,马轩,等.高效液相色谱法测定人造板中甲醛含量的新方法[J].林业工程学报,2015,29(6):109-112.Guo FY,Yu HX,Ma X,et al.Determination of formaldehyde in wood-based panels by high performance liquid chromatography[J].China Forest Sci Technol,2015,29(6):109-112.
[8]龙举,张小军,郭远明,等.高效液相色谱法测定海捕鱼中甲醛的含量[C].2013年浙江省渔业科技论坛论文集,2013.Long J,Zhang XJ,Guo YM,et al.Determination of formaldehyde in sea fish by high performance liquid chromatography[C].Collection of BBSPapers on Fishery Science and Technology of Zhejiang Province in 2013,2013.
[9]赵婷,赵梅,温正如,等.高效液相色谱法测定织物涂层整理剂中的甲醛含量[J].陕西科技大学学报(自然科学版),2009,27(2):69-72.Zhao T,Zhao M,Wen ZR,et al.Determination of formaldehyde content in textile coating agents by high performance liquid chromatography method[J].J Shaanxi Univ Sci Technol(Nat Sci Ed),2009,27(2):69-72.
[10]冯敏铃,李盛安.高效液相色谱法测定大白菜中甲醛残留效果研究[J].现代农业科技,2013,(9):281,284.Feng ML,Li SA.Determination of formaldehyde residue in Chinese cabbage by high performance liquid chromatography[J].Mod Agric Sci Technol,2013,(9):281,284.
[11]王圣庆,郭瑛,马言顺,等.柱前衍生高效液相色谱法测定啤酒中微量甲醛[J].化学研究与应用,2006,18(2):214-216.Wang SQ,Guo Y,Ma YS,et al.Determination of trace formaldehyde in beer by HPLC with precolumn derivatization and UV detection[J].Chem Res Appl,2006,18(2):214-216.
[12]甘凝岚,颜春荣,徐春祥,等.高效液相色谱法测定鸭血制品中甲醛含量[J].食品科学,2014,35(12):204-207.Gan NL,Yan CR,Xu CX,et al.Determination of formaldehyde in duck blood products by HPLC[J].Food Sci,2014,35(12):204-207.
[13]王帆,王勇,黄洁玉,等.纺织品中游离甲醛含量的高效液相色谱法测定[J].分析科学学报,2006,22(4):428-430.Wang F,Wang Y,Huang JY,et al.Determination of free formaldehyde in textiles by high performance liquid chromatography[J].J Anal Sci,2006,22(4):428-430.
[14]吴新华,朱瑞芝,陆舍铭,等.高效液相色谱法测定香精中甲醛的含量[J].化学试剂,2010,32(9):817-818,858.Wu XH,Zhu RZ,Lu SM,et al.Determination of formaldehyde in flavors using high performance liquid chromatography[J].Chem Reagent,2010,32(9):817-818,858.
[15]李向荣,黄亚羲.高效液相色谱法测定草酸二甲酯中甲醛含量[J].分析仪器,2013,(5):15-17.Li XR,Huang YX.Determination of formaldehyde in dimethyl oxalate by HPLC[J].Anal Instrum,2013,(5):15-17.
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |