高效液相色谱法快速测定怀药中的六价铬
Rapid Determination of Chromium(Ⅵ) in Huaiyao by HPLC
摘 要
采用高效液相色谱法测定怀药中六价铬的含量。样品经0.1 mol·L-1磷酸氢二钾溶液超声提取3次后,提取液再经磷酸(7+3)溶液-10 g·L-1的1,5-二苯卡巴肼溶液-300 g·L-1聚乙二醇溶液(1+1+10)的混合液超声萃取20 min后,分离得到聚乙二醇层,在Xterra ODS C18色谱柱上分离,以pH 2.5的0.1 mol·L-1磷酸氢二钾溶液-甲醇(57+43)混合液为流动相,于波长540 nm处进行测定。六价铬的质量浓度在4.0~400 μg·L-1范围内与峰面积呈线性关系,检出限(3S/N)为40 ng·L-1。加标回收率在98.9%~103%之间,测定值的相对标准偏差(n=5)小于2.0%。
六价铬
怀药
萃取
HPLC
Chromium(Ⅵ)
Huaiyao
Extraction
Abstract
HPLC was applied to the determination of chromium(Ⅵ) in Huaiyao. The sample was extracted with 0.1 mol·L-1 of KH2PO4 solution by ultralsonic for 3 times. The extract solution was extracted for 20 min by utralsonic with a mixture of phosphoric acid (7+3) solution, 10 g·L-1 of 1,5-diphenyl carbazide solution and 300 g·L-1 of polyethylene glycol solution. The polyethylene glycol layer was separated on an Xterra ODS C18 column, with a mixture of pH 2.5, 0.1 mol·L-1 KH2PO4 solution and methanol (57+43) as mobile phase. The detection wavelength was 540 nm. Linear relationship was found between the peak area and the mass concentration of chromium(Ⅵ) in the range of 4.0-400 μg·L-1, with detection limit (3S/N) of 40 ng·L-1. Values of recovery obtained by standard addition method were in the range of 98.9%-103%, and RSDs (n=5) were less than 2.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx201611014
所属栏目 工作简报
基金项目 焦作市软科学研究计划项目(SJC20130006;SRK20130001;SRK20140008)
收稿日期 2015/11/1
修改稿日期
网络出版日期
作者单位点击查看
联系人作者周桂友(gychow@163.com)
备注侯艳芳(1980-),女,河南焦作人,农艺师,硕士,主要从事农产品理化分析工作。
引用该论文: HOU Yan-fang,ZHOU Gui-you. Rapid Determination of Chromium(Ⅵ) in Huaiyao by HPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2016, 52(11): 1306～1309
侯艳芳,周桂友. 高效液相色谱法快速测定怀药中的六价铬[J]. 理化检验－化学分册, 2016, 52(11): 1306～1309
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参考文献
【1】张云,陈晓燕.地表水环境中六价铬的测定研究[J].应用化工, 2012,41(2):349-351.
【2】张星刚,肖新峰,张强.聚乙二醇双水相萃取光度法测定铬(Ⅵ)[J].分析试验室, 2010,29(6):105-107.
【3】GB/T 22807-2008皮革和毛皮 化学试验 六价铬含量的测定[S].
【4】YING L Y, JIANG H L, ZHOU S C, et al. Ionic liquid as a complexation and extraction medium combined with high-performance liquid chromatography in the evaluation of chromium(Ⅵ) and chromium(Ⅲ) speciation in wastewater samples[J]. Microchemical Journal, 2011,98(2):200-203.
【5】周桂友,侯艳芳,封琳,等.反相高效液相色谱法测定陶瓷饰品中六价铬的溶出量[J].理化检验-化学分册, 2015,51(1):86-90.
【6】CHEN S J, ZHANG X S, YU L Y, et al. Simultaneous determination of Cr(Ⅲ) and Cr(Ⅵ) in tannery wastewater using low pressure ion chromatography combined with flow injection spectrophotometry[J]. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2012,88:49-55.
【7】张涛,蔡五田,刘金巍,等.超声辅助提取/离子色谱法测定铬污染土壤中的六价铬[J].分析测试学报, 2013,32(11):1384-1387.
【8】虞锐鹏,胡忠阳,叶明立,等.快速溶剂萃取-离子色谱法同时测定塑料中的三价铬和六价铬[J].色谱, 2012,30(4):409-413.
【9】茅文良,汪磊,张克和,等.HPLC法测定纺织品中可萃取六价铬[J].印染, 2011,37(14):37-39.
【10】沈兵,王练,奚奇辉,等.高效液相色谱法测定皮革中的六价铬[J].中国皮革, 2008,37(11):39-41.
【11】ANDREA N, EDINA B, ATTILA G. Interfacing microfluidic chip-based chromatography with flame atomic absorption spectrometry for the determination of chromium(Ⅵ)[J]. Microchemical Journal, 2014,114:216-222.
【12】NAO K, TETSUO I, MASARU K, et al. Determination of chromium(Ⅲ), chromium(Ⅵ), and chromium(Ⅲ) acetylacetonate in water by ion-exchange disk extraction/metal furnace atomic absorption spectrometry[J]. Spectrochimica Acta Part B: Atomic Spectroscopy, 2014,93:28-33.
【13】SUSAN S, ALI Z M. Preconcentration and speciation of trace amounts of chromium in saline samples using temperature-controlled microextraction based on ionic liquid as extraction solvent and determination by electrothermal atomic absorption spectrometry[J]. Talanta, 2012,99(15):758-766.
【14】RYSZARD D, LWONA P, JOANNA D, et al. Chromium determination in food by slurry sampling graphite furnace atomic absorption spectrometry using classical and permanent modifiers[J], Food Chemistry, 2012,132(1):597-602.
【15】肖亚兵,吴延晖,张曼,等.石墨炉原子吸收法直接测定鸡蛋中的六价铬[J].分析测试学报, 2007,26(2):235-238.
【16】BARBARA M, LZABELA K, ADAM S, et al. Chromium and its speciation in water samples by HPLC/ICP-MS-technique establishing metrological traceability: a review since 2000[J]. Talanta, 2015,132:814-828.
【17】CHEN S Z, ZHU S P, HE Y Y, et al. Speciation of chromium and its distribution in tea leaves and tea infusion using titanium dioxide nanotubes packed microcolumn coupled with inductively coupled plasma mass spectrometry[J]. Food Chemistry, 2014,150:254-259.
【18】MAGDALENA S, BEATA J, WOJCIECH W. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace[J]. Talanta, 2013,117:14-19.
【19】郭少飞,王鹏,王帆,等.高效液相色谱-电感耦合等离子体质谱法测定粉质化妆品中的六价铬[J].检验检疫学刊, 2012,22(4):8-13.
【20】王骏,胡梅,张卉,等.液相色谱-质谱法对饮用水中六价铬的测定[J].分析测试学报, 2009,28(12):1468-1470.
【2】张星刚,肖新峰,张强.聚乙二醇双水相萃取光度法测定铬(Ⅵ)[J].分析试验室, 2010,29(6):105-107.
【3】GB/T 22807-2008皮革和毛皮 化学试验 六价铬含量的测定[S].
【4】YING L Y, JIANG H L, ZHOU S C, et al. Ionic liquid as a complexation and extraction medium combined with high-performance liquid chromatography in the evaluation of chromium(Ⅵ) and chromium(Ⅲ) speciation in wastewater samples[J]. Microchemical Journal, 2011,98(2):200-203.
【5】周桂友,侯艳芳,封琳,等.反相高效液相色谱法测定陶瓷饰品中六价铬的溶出量[J].理化检验-化学分册, 2015,51(1):86-90.
【6】CHEN S J, ZHANG X S, YU L Y, et al. Simultaneous determination of Cr(Ⅲ) and Cr(Ⅵ) in tannery wastewater using low pressure ion chromatography combined with flow injection spectrophotometry[J]. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2012,88:49-55.
【7】张涛,蔡五田,刘金巍,等.超声辅助提取/离子色谱法测定铬污染土壤中的六价铬[J].分析测试学报, 2013,32(11):1384-1387.
【8】虞锐鹏,胡忠阳,叶明立,等.快速溶剂萃取-离子色谱法同时测定塑料中的三价铬和六价铬[J].色谱, 2012,30(4):409-413.
【9】茅文良,汪磊,张克和,等.HPLC法测定纺织品中可萃取六价铬[J].印染, 2011,37(14):37-39.
【10】沈兵,王练,奚奇辉,等.高效液相色谱法测定皮革中的六价铬[J].中国皮革, 2008,37(11):39-41.
【11】ANDREA N, EDINA B, ATTILA G. Interfacing microfluidic chip-based chromatography with flame atomic absorption spectrometry for the determination of chromium(Ⅵ)[J]. Microchemical Journal, 2014,114:216-222.
【12】NAO K, TETSUO I, MASARU K, et al. Determination of chromium(Ⅲ), chromium(Ⅵ), and chromium(Ⅲ) acetylacetonate in water by ion-exchange disk extraction/metal furnace atomic absorption spectrometry[J]. Spectrochimica Acta Part B: Atomic Spectroscopy, 2014,93:28-33.
【13】SUSAN S, ALI Z M. Preconcentration and speciation of trace amounts of chromium in saline samples using temperature-controlled microextraction based on ionic liquid as extraction solvent and determination by electrothermal atomic absorption spectrometry[J]. Talanta, 2012,99(15):758-766.
【14】RYSZARD D, LWONA P, JOANNA D, et al. Chromium determination in food by slurry sampling graphite furnace atomic absorption spectrometry using classical and permanent modifiers[J], Food Chemistry, 2012,132(1):597-602.
【15】肖亚兵,吴延晖,张曼,等.石墨炉原子吸收法直接测定鸡蛋中的六价铬[J].分析测试学报, 2007,26(2):235-238.
【16】BARBARA M, LZABELA K, ADAM S, et al. Chromium and its speciation in water samples by HPLC/ICP-MS-technique establishing metrological traceability: a review since 2000[J]. Talanta, 2015,132:814-828.
【17】CHEN S Z, ZHU S P, HE Y Y, et al. Speciation of chromium and its distribution in tea leaves and tea infusion using titanium dioxide nanotubes packed microcolumn coupled with inductively coupled plasma mass spectrometry[J]. Food Chemistry, 2014,150:254-259.
【18】MAGDALENA S, BEATA J, WOJCIECH W. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace[J]. Talanta, 2013,117:14-19.
【19】郭少飞,王鹏,王帆,等.高效液相色谱-电感耦合等离子体质谱法测定粉质化妆品中的六价铬[J].检验检疫学刊, 2012,22(4):8-13.
【20】王骏,胡梅,张卉,等.液相色谱-质谱法对饮用水中六价铬的测定[J].分析测试学报, 2009,28(12):1468-1470.
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