固相萃取分离-高效液相色谱法测定陈皮中噻菌灵残留量
HPLC Determination of Residual Amount of Thiabendazole in Dried Tangerine After Separation by SPE and Ion-exchange
摘 要
试样于磷酸(1+999)溶液中浸泡2 h,超声振荡20 min,加水定容为50 mL离心3 min,分取上层澄清液5.0 mL,通过ENVITM C18固相萃取柱纯化.用由0.1 mol·L-1磷酸二氢钾溶液(pH 3.0)与乙腈以70比30的体积比组成的混合液(此溶液也用作流动相)作为淋洗液,将被测定物质从固相萃取柱上洗脱,所得淋出液供高效液相色谱(HPLC)测定.HPLC分析中,LC-SCX离子交换柱用作色谱柱,上述的混合溶液作为流动相,荧光检测的激发波长为307 nm,发射波长为359 nm.噻菌灵的质量浓度在0.5~100.0 μg·L-1范围内与其相应的峰面积值之间呈线性关系,在3个浓度水平上对回收率作了试验,测得回收率在88.0%~95.0%之间,相对标准偏差(n=6)在3.1%~5.0%之间.
离子交换色谱柱
荧光检测
噻菌灵
陈皮
HPLC
Ion-exchange chromatographic column
Fluorescence detection
Thiabendazole
Dried tangerine
Abstract
Sample was soaked with dil.H3PO4 (1+999) solution for 2 h,agitated for 20 min ultrasonically and centrifuged for 3 min after diluting to 50 mL.An aliquot of the supernatant solution was taken for purification by passing through the ENVITM C18 SPE column.A mixed solution,containing 0.1 mol·L-1 KH2PO4 of pH 3.0 and acetonitrile mixed in the ratio of 70 to 30 by volume (which was also used as mobile phase) was used as eluant to elute the analyte from the SPE column,and the eluate obtained was used for HPLC determination.The LC-SCX column was used as ion-exchange chromatographic column and the mixed solution mentioned above was used as mobile phase in the HPLC analysis with fluorescence detection at the wavelengths of 307 nm (λex) and 359 nm (λem).Range of linearity was found in the concentration range of 0.5-100.0 μg·L-1 of thiabendazole against values of relative peak area.Test for recovery was performed at 3 concentration levels,giving values of av.recovery in the range of 88.0%-95.0% and RSD′s (n=6) in the range 3.1%-5.0%.
中图分类号 O657.37
所属栏目 工作简报
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收稿日期 2007/12/11
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备注赵洁(1981-),女,陕西西安人,硕士,助教,主要研究方向为药物分析.
引用该论文: ZHAO Jie,HE Qiang,KONG Xiang-hong,LI Jian-hua. HPLC Determination of Residual Amount of Thiabendazole in Dried Tangerine After Separation by SPE and Ion-exchange[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(2): 215～217
赵洁,何强,孔祥虹,李建华. 固相萃取分离-高效液相色谱法测定陈皮中噻菌灵残留量[J]. 理化检验－化学分册, 2009, 45(2): 215～217
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参考文献
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【6】Orea J M,Bescos B,Montero C,et al.Analysis of carbendazim in agricultural samples by laser desorption and REMPI time-of-flight mass spectrometry[J].Anal Chem,1998,70(3):491．
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