色谱

色谱

• 技术与应用 • 上一篇    

在线柱浓缩-超高效液相色谱法测定水体中的痕量甲萘威和呋喃丹

王恩智1, 杨新磊2, 叶明立2, 汪琼2, 蔡小军3*   

  1. 1. 台州市中西医结合医院(泽国院区), 浙江 温岭 317523; 2. 戴安中国有限公司应用研究中心上海实验室, 上海 201203; 3. 温州医学院药学院, 浙江 温州 325035
  • 收稿日期:2011-05-19 修回日期:2011-08-06 出版日期:2011-11-28 发布日期:2011-12-25
  • 通讯作者: 蔡小军,硕士,主要从事测试分析方法开发
  • 基金资助:

    浙江省自然科学基金项目(Nos. R4080124, Y507252)和浙江省分析测试基金项目(No. 2007F70061)

Determination of trace carbaryl and carbofuran in water by online column enrichment-ultra high performance liquid chromatography

WANG Enzhi1, YANG Xinlei2, YE Mingli2, WANG Qiong2, CAI Xiaojun3*   

  1. 1. Taizhou Hospital of Integrated Traditional and Western Medicine (Zeguo District), Wenling 317523, China; 2. Shanghai Laboratory of Application and Research Center, Dionex China Limited, Shanghai 201203, China; 3. School of Pharmacy, Wenzhou Medical College, Wenzhou 325035, China
  • Received:2011-05-19 Revised:2011-08-06 Online:2011-11-28 Published:2011-12-25

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摘要： 采用在线柱浓缩-超高效液相色谱联用技术测定水体中痕量甲萘威和呋喃丹。水样过滤后直接进样,采用固相萃取小柱富集待测物,梯度洗脱后,利用阀切换技术将待测物反冲至分析柱Acclaim RSLC C18(100 mm×2.1 mm, 2.2 μm)上进行色谱分离,以10 mmol/L醋酸铵缓冲溶液(pH 5.0,用醋酸调节)和乙腈分别为流动相A和B,梯度洗脱,泵流速为0.8 mL/min,检测波长为280 nm,二极管阵列检测器检测。甲萘威和呋喃丹在1.0～100 μg/L范围内线性良好(相关系数r2 ＞ 0.9999),检出限(S/N=3)分别为0.5和0.25 μg/L,加标回收率为76.0%～120.0%。用所建立的方法测定了水中痕量的甲萘威与呋喃丹的含量,结果令人满意。

关键词: 超高效液相色谱, 呋喃丹, 甲萘威, 双梯度, 在线柱浓缩

Abstract: An online column enrichment-ultra high performance liquid chromatography (UHPLC) method was developed to determine trace carbaryl and carbofuran in water. The sample was injected into a UHPLC system directly after filtration with 0.22 μm membrane, and then enriched by online solid phase extraction (SPE) column. The analyte was back-flushed into the analytical column Acclaim RSLC C18 (100 mm×2.1 mm, 2.2 μm) by valve switching method. The mobile phases were 10 mmol/L ammonium acetate buffer (pH 5.0, adjusted by acetic acid) and acetonitrile in a gradient elution mode with a flow rate of 0.8 mL/min, and detected by a diode array detector with the detection wavelength of 280 nm. The good linear ranges of carbaryl and carbofuran were 1.0~100 μg/L with the correlation coefficients (r2) larger than 0.9999, and the limits of detection (S/N=3) were 0.5 μg/L and 0.25 μg/L, respectively. The average spiked recoveries were in the range of 76.0%~120.0%. The method has been applied to determine trace carbaryl and carbofuran in water samples with satisfactory results.

Key words: carbaryl, carbofuran, online column enrichment, ultra high performance liquid chromatography (UHPLC), dual gradient