HPLC和LC-IT-TOF测定“地沟油”中DBS方法的建立
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殷果女副主任药师,研究方向为药品质量标准研究E-mail:ayinguoa@126.com

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Development of HPLC determination and LC-IT-TOF verification of DBS in gutter oil
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    摘要:

    建立“地沟油”中十二烷基苯磺酸钠(DBS)的测定和验证。方法样品经50%乙醇提取,经固相萃取柱纯化,采用高效液相色谱法(HPLC)测定其中的DBS含量,色谱柱为Nucleodur C18柱(250mm×4.6mm×5μm),流动相为甲醇∶乙酸铵(10mmol/L)=80∶20,流速为1.0ml/min,检测波长为244nm。并采用LC-IT-TOF进行验证,质谱离子化模式ESI-,雾化气流速1.5L/min,检测器电压1.68kV。结果在4.030~503.3μg/ml浓度范围内,DBS可被准确测定,回收率为77%~87%,精密度RSD% 均<2.0%。7批“地沟油”样品和23批非“地沟油”样品验证结果与测定结果相同。结论本研究建立的测定和验证方法均符合要求,可应用于“地沟油”中DBS的测定和测定结果验证。

    Abstract:

    To develop a determination and verification method for DBS in gutter oil and its application. Methods After extracted by 50% ethanol and purified by SPE column, the DBS in gutter oil was detected by HPLC, separated by a Nucleodur C18 column(250mm×4.6mm×5μm) with mobile phase consisting of methanol (containing 20% 10mmol/L ammonium acetate). Verification was operated by LC-IT-TOF mass spectroscopy in ESI-ionization model, nebulizing gas was 1.5ml/min and detector voltage was 1.68kV. ResultsQuantity of DBS in gutter oil was accuratly determined in the range of 4.030-503.3μg/ml, the recoveries were 77%-87% and RSD% of precision was less than 2%. All 7batches of gutter oils and 23batches of edible oils matched the results of verification. Conclusion The method was suitable for the detection of DBS in gutter oil.

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殷果,鲁艺,谢普,李媛,王铁杰. HPLC和LC-IT-TOF测定“地沟油”中DBS方法的建立[J].中国食品卫生杂志,2013,25(1):37-39.

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  • 收稿日期:2012-07-11
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