离子色谱法测定豇豆和苦瓜中对氯苯氧乙酸的残留量
IC Determination of Residual Amount of 4-Chlorophenoxyacetic Acid in Cowpea and Bitter Gourd
摘 要
采用离子色谱法测定豇豆和苦瓜中对氯苯氧乙酸的残留量。豇豆和苦瓜样品采用1.8 mmol·L-1碳酸钠-1.7 mmol·L-1碳酸氢钠溶液超声提取，固相萃取C18小柱净化。以1.8 mmol·L-1碳酸钠-1.7 mmol·L-1碳酸氢钠溶液为流动相，紫外检测器测定。对氯苯氧乙酸的质量浓度在0.05~25.0 mg·L-1内与其对应的峰面积呈线性关系，对氯苯氧乙酸在豇豆和苦瓜中的检出限（3S/N）依次为0.04，0.03 mg·kg-1。以空白样品为基体进行加标回收试验，所得回收率在96.7%~109%之间，测定值的相对标准偏差（n=5）在4.7%~7.7%之间。
对氯苯氧乙酸
豇豆
苦瓜
IC
4-chlorophenoxyacetic acid
cowpea
bitter gourd
Abstract
IC was applied to the determination of residual amount of 4-chlorophenoxyacetic acid in cowpea and bitter gourd. The sample of cowpea and bitter gourd was extracted ultrasonically with mixture of 1.8 mmol·L-1 Na2CO3 and 1.7 mmol·L-1 NaHCO3 solution, and then purified with SPE C18 colunm. Mixture of 1.8 mmol·L-1 Na2CO3 and 1.7 mmol·L-1 NaHCO3 solution was used as mobile phase,and UV detector was used in determination. Linear relationship between values of peak area and mass concentration of 4-chlorophenoxyacetic acid was kept in the range of 0.05-25.0 mg·L-1, with detection limits (3S/N) in cowpea and bitter gourd of 0.04, 0.03 mg·kg-1 respectively. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 96.7%-109%, with RSD's (n=5) in the range of 4.7%-7.7%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201705024
所属栏目 专题报道
基金项目 国家重大科学仪器设备开发专项（2012YQ09022910）；海南省自然科学基金（214019）
收稿日期 2016/4/22
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联系人作者章程辉(zchlm@163.com)
备注谢艳丽(1976-),女,河南洛阳人,高级实验师,主要从事色谱研究工作
引用该论文: XIE Yanli,ZHAO Zhendong,FENG Yuhong,ZHANG Chenghui. IC Determination of Residual Amount of 4-Chlorophenoxyacetic Acid in Cowpea and Bitter Gourd[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(5): 594～597
谢艳丽,赵振东,冯玉红,章程辉. 离子色谱法测定豇豆和苦瓜中对氯苯氧乙酸的残留量[J]. 理化检验－化学分册, 2017, 53(5): 594～597
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参考文献
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【11】贾娜,韩梅,李科,等.离子色谱-电感耦合等离子体质谱法测定地下水中4种形态砷的含量[J].理化检验-化学分册, 2016,52(3):292-295.
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【2】SINGH H K, SAQUIB M, HAQUE M M, et al.Heterogeneous photocatalysed degradation of 4-chlorophenoxyacetic acid in aqueous suspensions[J]. Journal of Hazardous Materials, 2007,142(1/2):374-380.
【3】FU F F, XIAO L X, WANG W, et al. Study on the degradation of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chloro-phenoxyacetic sodium (MCPA sodium) in natural agriculture-soils of Fuzhou[J]. Science of The Total Environment, 2009,407(6):1998-2003.
【4】彭敏,刘传生.固相萃取-柱前衍生-气相色谱-质谱联用法测定水中2,4-滴和灭草松[J].理化检验-化学分册, 2009,45(7):791-793.
【5】匡华,储晓刚,侯玉霞,等.气相色谱法同时测定大豆中13种苯氧羧酸类除草剂的残留量[J].中国食品卫生杂志, 2006,18(6):503-508.
【6】冯家望,吴洁珊,曹桂云,等.高效液相色谱-串联质谱法测定食品中对氯苯氧乙酸的残留量[J].理化检验-化学分册, 2012,48(10):1219-1221.
【7】钟莉萍,徐敦明,方恩华,等.高效液相色谱法和高效液相色谱-质谱/质谱法测定荔枝中对氯苯氧乙酸(钠)[J].检验检疫学刊, 2010年,20(2):24-27.
【8】潘雪峰,陈樱玉.对氯苯氧乙酸液相色谱分析[J].现代农药, 2011,10(2):30-31.
【9】王一茜,张广华,赵学志,等.对氯苯氧乙酸钠在绿豆芽中的残留量分析[J].食品科技, 2013,38(10):316-319.
【10】戴达勇,杨英桂,贺万鑫.离子色谱法同时测定沙棘果粉中7种有机酸含量[J].理化检验-化学分册, 2015,51(3):304-306.
【11】贾娜,韩梅,李科,等.离子色谱-电感耦合等离子体质谱法测定地下水中4种形态砷的含量[J].理化检验-化学分册, 2016,52(3):292-295.
【12】GUO D D, LOU C Y, ZHANG P M, et al. Polystyrene-divinylbenzene-glycidyl methacrylate stationary phase grafted with poly (amidoamine) dendrimers for ion chromatography[J]. Journal of Chromatography A, 2016,1456:113-122.
【13】NI C Z, ZHU B H, WANG N N, et al. Simple column-switching ion chromatography method for determining eight monosaccharides and oligosaccharides in honeydew and nectar[J]. Food Chemistry, 2016,194:555-560.
【14】JIANG Z Z, WANG Y F, CHEN R R. Rapid analysis of volatile fatty acids in feces by headspace gas chromatography tandem mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2014,42(3):429-435.
【15】裘亚均,徐育,张佑球,等.离子色谱法电导检测测定土壤中的对氯苯氧乙酸[J].宁波高等专科学校学报, 2001,13(增1):155-158.
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