反相高效液相色谱法测定陶瓷饰品中六价铬的溶出量
Determination of Chromium(Ⅵ) Released from Ceramic Jewelry by Reversed-Phase HPLC
摘 要
提出了柱前衍生反相高效液相色谱法测定陶瓷饰品中六价铬溶出量的方法。采用人工汗液萃取陶瓷饰品,用1,5-二苯卡巴肼与萃取液中的六价铬在酸性条件下进行衍生反应,衍生物在Waters SunFire ODS C18色谱柱上分离,以pH 2.5的10 mmol·L-1磷酸二氢钾缓冲溶液和丙酮为流动相进行梯度洗脱,于波长540 nm处进行测定。六价铬的质量浓度在5.0~200.0 μg·L-1范围内与峰面积呈线性关系,相关系数为0.999 1,检出限(3S/N)为0.037 μg·L-1。空白(实际样品)的加标回收率在97%~101%之间,测定值的相对标准偏差在1.9%~3.2%之间。
六价铬
陶瓷饰品
Reversed-phase HPLC
Chromium(Ⅵ)
Ceramic jewelry
Abstract
The reversed-phase high performance liquid chromatography (RP-HPLC) combined with pre-column derivatization was used to determine chromium(Ⅵ) released from ceramic jewelry. The ceramic jewelry sample was extracted by artificial sweat. Chromium(Ⅵ) in the extraction was derivatized with 1,5-diphenylcarbazide under acidic condition. The derivative was separated using Waters SunFire ODS C18 column as stationary phase and a mixture of acetone and KH2PO4 solution of 10 mmol·L-1 with pH 2.5 as mobile phase for gradient elution. Absorbance at 540 nm was measured. The linear relationship between the peak area and the mass concentration of chromium(Ⅵ) was found in the range of 5.0-200.0 μg·L-1, with correlation coefficient of 0. 999 1 and detection limit (3S/N) of 0.037 μg·L-1. Tests for recovery were made by standard addition, giving recovery rates in the range of 97%-101% and RSD (n=7) in the range of 1.9%-3.2%.
中图分类号 O652.63
所属栏目 工作简报
基金项目
收稿日期 2013/12/23
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)
备注周桂友(1981-),男,山东临沂人,工程师,硕士,主要从事理化分析工作。
引用该论文: ZHOU Gui-you,HOU Yan-fang,FENG Lin,YU Jian. Determination of Chromium(Ⅵ) Released from Ceramic Jewelry by Reversed-Phase HPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(1): 86～90
周桂友,侯艳芳,封琳,虞舰. 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
被引情况:
【1】侯艳芳,周桂友, "高效液相色谱法快速测定怀药中的六价铬",理化检验－化学分册 52, 1306-1309(2016)
【2】陶小美,胡爱生,朱杰杨, "高效液相色谱-电感耦合等离子体质谱法测定玩具材料中六价铬",理化检验－化学分册 52, 1451-1453(2016)
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参考文献
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【2】YING Li-yan, JIANG Hai-liang, ZHOU Sai-sun, 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.
【3】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.
【4】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.
【5】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.
【6】ESPADA-BELLIDO E, BI Zhao-shun, VAN DEN BERG C M G. Determination of chromium in estuarine waters by catalytic cathodic stripping voltammetry using a vibrating silver amalgam microwire electrode［J］. Talanta, 2013,105:287-291.
【7】ZHANG Hai-yan, LIU Qian, WANG Thanh, et al. Facile preparation of glutathione-stabilized gold nanoclusters for selective determination of chromium(Ⅲ) and chromium(Ⅵ) in environmental water samples［J］. Anal Chim Acta, 2013,770:140-146.
【8】EI-SHAHAWI M S, AI-SAIDI H M, BASHAMMAKH A S, et al. Spectrofluorometric determination and chemical speciation of trace concentrations of chromium (Ⅲ & Ⅵ) species in water using the ion pairing reagent tetraphenyl-phosphonium bromide［J］. Talanta, 2011,84(1):175-179.
【9】CHEN Shu-juan, ZHANG Xin-shen, YU Ling-yun, 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.
【10】PASTORE P, FAVARO G, BALLARDIN A, et al. Evidence of Cr(Ⅵ) formation during analysis of leather proposal of an alternative method of analysis through the ion-chromatographic approach and post-column reaction［J］. Talanta, 2004,63(4):941-947.
【11】SADEGHI S, MOGHADDAM A Z. 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, 2012,99:758-766.
【12】DOBROWOLSKI R, PAWLOWSKA-KAPUSTA I, DOBRZYNSKA J, 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.
【13】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.
【14】邓琴,黄文耀.食品中六价铬的测定［J］.中国卫生检验杂志, 2010,20(11):2759-2760.
【15】HOTTA H, YATA K, KAMARUDIN K F B, et al. Determination of chromium(Ⅲ), chromium(Ⅵ) and total chromium in chromate and trivalent chromi-um conversion coatings by electrospray ionization mass spectrometry［J］. Talanta, 2012,88:533-536.
【16】MENG Qing-yu, FAN Zhi-hua, BUCKLEY B, et al. Development and evaluation of a method for hexavalent chromium in ambient air using IC-ICP-MS［J］. Atmospheric Environment, 2011,45(12):2021-2027.
【17】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.
【18】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.
【19】GB/T 22807-2008皮革和毛皮 化学试验 六价铬含量的测定［S］.
【20】GB/T 3922-1995纺织品耐汗渍色牢度试验方法［S］.
【21】GB/T 3534-2002日用陶瓷器铅、镉溶出量的测定方法［S］.
【2】YING Li-yan, JIANG Hai-liang, ZHOU Sai-sun, 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.
【3】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.
【4】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.
【5】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.
【6】ESPADA-BELLIDO E, BI Zhao-shun, VAN DEN BERG C M G. Determination of chromium in estuarine waters by catalytic cathodic stripping voltammetry using a vibrating silver amalgam microwire electrode［J］. Talanta, 2013,105:287-291.
【7】ZHANG Hai-yan, LIU Qian, WANG Thanh, et al. Facile preparation of glutathione-stabilized gold nanoclusters for selective determination of chromium(Ⅲ) and chromium(Ⅵ) in environmental water samples［J］. Anal Chim Acta, 2013,770:140-146.
【8】EI-SHAHAWI M S, AI-SAIDI H M, BASHAMMAKH A S, et al. Spectrofluorometric determination and chemical speciation of trace concentrations of chromium (Ⅲ & Ⅵ) species in water using the ion pairing reagent tetraphenyl-phosphonium bromide［J］. Talanta, 2011,84(1):175-179.
【9】CHEN Shu-juan, ZHANG Xin-shen, YU Ling-yun, 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.
【10】PASTORE P, FAVARO G, BALLARDIN A, et al. Evidence of Cr(Ⅵ) formation during analysis of leather proposal of an alternative method of analysis through the ion-chromatographic approach and post-column reaction［J］. Talanta, 2004,63(4):941-947.
【11】SADEGHI S, MOGHADDAM A Z. 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, 2012,99:758-766.
【12】DOBROWOLSKI R, PAWLOWSKA-KAPUSTA I, DOBRZYNSKA J, 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.
【13】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.
【14】邓琴,黄文耀.食品中六价铬的测定［J］.中国卫生检验杂志, 2010,20(11):2759-2760.
【15】HOTTA H, YATA K, KAMARUDIN K F B, et al. Determination of chromium(Ⅲ), chromium(Ⅵ) and total chromium in chromate and trivalent chromi-um conversion coatings by electrospray ionization mass spectrometry［J］. Talanta, 2012,88:533-536.
【16】MENG Qing-yu, FAN Zhi-hua, BUCKLEY B, et al. Development and evaluation of a method for hexavalent chromium in ambient air using IC-ICP-MS［J］. Atmospheric Environment, 2011,45(12):2021-2027.
【17】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.
【18】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.
【19】GB/T 22807-2008皮革和毛皮 化学试验 六价铬含量的测定［S］.
【20】GB/T 3922-1995纺织品耐汗渍色牢度试验方法［S］.
【21】GB/T 3534-2002日用陶瓷器铅、镉溶出量的测定方法［S］.
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