Spectrophotometric Determination of Cadmium in Edible Fungi with Separation by Dispersive Liquid-Liquid Microextraction
摘 要
取经清洗、粉碎并烘干的样品0.500 0 g,用硝酸5 mL及过氧化氢3 mL,按程序升温模式微波消解。消解液于沸水浴中蒸发至约1 mL,用水定容至50 mL。取此溶液5.00 mL依次加入0.2 g·L-1 5-Br-PADAP溶液2.0 mL,氨性缓冲溶液(pH 9.0)3.0 mL及100 g·L-1 Triton X-114溶液3.0 mL,加水定容至25 mL,摇匀,使Cd2+生成络合物,10 min后加入辛醇1.0 mL,涡旋混合1 min,离心5 min,吸出下层溶液,取出上层红色有机层,用乙醇定容至3 mL,于540 nm处用1 cm比色皿测得其吸光度。镉的质量浓度在10.00 mg·L-1以内与吸光度呈线性关系,检出限(3s)为0.05 mg·L-1。加标回收率为93.3%~103%,测定值的相对标准偏差(n=6)小于5.0%。
Abstract
0.500 0 g of the cleaned, crushed and dried sample was digested with HNO3 (5 mL) and H2O2 (3 mL) in microwave oven under the mode of programmed temperature elevation. After digestion, the sample solution was evaporated to about 1 mL in boiling water bath, and then water was added to make up its volume to 50 mL. 5.00 mL of the solution was taken and the following solutions were added in succession:1 0.2 g·L-1 5-Br-PADAP:2.0 mL; 2 ammoniacal buffer (pH 9.0):3.0 mL; and 3 100 g·L-1 Triton X-114:3.0 mL。Then the volume was made up to 25 mL with water and mixed thorough to have the colored complex of Cd2+ formed. After 10 min, 1.0 mL of octyl alcohol was added and swirled for 1 min. After centrifugation for 5 min and phase separation, the lower phase was removed and the red colored upper phase was taken and made up its volume to 3 mL with ethyl alcohol. The absorbance of the red solution was measured at 540 nm. Linearity for Cd2+ was kept in the range within 10.00 mg·L-1, and the detection limit (3s) found was 0.05 mg·L-1. Values of recovery obtained by standard addition method were in the range of 93.3% to 103%. Values of RSDs (n=6) found were less than 5.0%.
中图分类号 O657.32 DOI 10.11973/lhjy-hx201712008
所属栏目 工作简报
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收稿日期 2016/11/28
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联系人作者杨亚玲(yilyil8@163.com)
备注李姌(1964-),女,云南昆明人,研究方向为生物及化学试验研究
引用该论文: LI Ran,WANG Meng,YANG Yaling. Spectrophotometric Determination of Cadmium in Edible Fungi with Separation by Dispersive Liquid-Liquid Microextraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(12): 1403~1406
李姌,王蒙,杨亚玲. 分散液液微萃取-分光光度法测定食用菌中镉的含量[J]. 理化检验-化学分册, 2017, 53(12): 1403~1406
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【3】丁月云,余大华,孟云,等.中草药复方对猪常见致病菌的体外抑菌试验[J].江苏农业科学, 2013,41(11):236-238.
【4】邹盛勤,陈武.食用菌的营养成分药理作用及开发利用[J].安徽农业科学, 2005,33(3):502-503.
【5】黄晨阳,张金霞.食用菌中重金属污染物含量的研究进展[J].中国食用菌, 2004,23(4):7-8.
【6】徐丹先,林佶,万玉萍,等.云南省常见野生食用菌镉含量调查分析[J].中国卫生检验杂志, 2011,21(3):705-707.
【7】李昌明,魏祖安,李文华,等.石墨炉原子吸收法快速连续监测柳江水中镉[J].中国卫生检验杂志, 2012,22(6):1298-1300.
【8】朱振科,陈建国,金献忠,等.可溶性滤膜分离富集电感耦合等离子体原子发射光谱法对水中痕量镉铜铅与锌的同时测定[J].分析测试学报, 2010,29(6):599-602.
【9】陈明丽,付海阔,孟皓,等.离子液体双水相萃取蒸气发生原子荧光法测定痕量镉[J].分析化学, 2010,38(9):1299-1304.
【10】于秀兰,田松涛,孟凡金.三氮烯类试剂在光度分析中的应用进展[J].岩矿测试, 2011,30(2):131-137.
【11】陈文宾,殷磊,斯琴高娃.1-(4-安替比林)-3-(3-硝基苯胺)三氮烯分光光度法测定镉(Ⅱ)[J].理化检验-化学分册, 2011,47(9):1043-1045.
【12】董学畅,郑永军,郝南明,等.固相萃取光度法测定环境水样中镉(Ⅱ)的研究[J].云南大学学报(自然科学版), 2005,27(3):235-238.
【13】MOHAMED G G, EI-BINDARY A A, RIZK M S. Extractive spectrophotometric method for determination of cadmium(Ⅱ) in different water sources[J]. Journal of Molecular Liquids, 2015,212:517-523.
【14】KODURU J R, LEE K D. Evaluation of thiosemicarbazone derivative as chelating agent for the simultaneous removal and trace determination of Cd(Ⅱ) and Pb(Ⅱ) in food and water samples[J]. Food Chemistry, 2014,150:1-8.
【15】曹江平,解启龙,周继梅,等.分散液液微萃取技术在食品分析中的应用进展[J].分析测试学报, 2015,34(5):616-624.
【16】高琳,陈圣洁,陈芳.Triton X-114存在下镉试剂分光光度法测定环境水样中的镉[J].岩矿测试, 2013,32(1):114-118.
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