液液萃取—固相萃取氣相色譜法測定火腿中有機磷農藥殘留量

蔣露 梅文泉 紹金良 賀玲

摘要 [目的]建立火腿中多種有機磷農藥殘留量同時測定的方法。[方法]火腿中有機磷農藥經乙腈提取后，用乙腈-正己烷液液萃取除去脂類和色素，再經石墨碳黑固相萃取小柱凈化，氣相色譜-火焰光度檢測器（GC-FPD）測定。[結果]16種有機磷農藥在DB-17、DB-1色譜柱上均獲得良好分離，在0.05～1.00 μg/mL范圍內，農藥殘留量色譜分析的線性關系良好，滿足定量分析要求，加標水平為0.08和0.20 mg/kg時，農藥的平均回收率在71.96%～117.21%，變異系數為1.73%～12.84%。方法的檢出限為0.005 3～0.011 8 mg/kg。[結論]該方法具有前處理簡單、凈化效果好、方法準確、靈敏度高、雜質干擾少的特點，適合火腿中有機磷農藥殘留量的分析。

關鍵詞 火腿；液液萃取；固相萃取；氣相色譜；有機磷農藥

中圖分類號 TS207.5+3 文獻標識碼 A 文章編號 0517-6611（2017）13-0092-04

Determination of Organophosphate Pesticide Residues in Ham Using Liquid-liquid Extraction / Solid-Phase Extraction with Gas Chromatography

JIANG Lu1， MEI Wen-quan2， SHAO Jin-liang2 et al

（1. The Agricultural-food Quality and Safety Center of Kunming， Kunming， Yunnan 650118； 2. Quality Standardizing and Testing Technology Institute， Yunnan Academy of Agricultural Sciences， Kunming， Yunnan 650223）

Abstract [Objective] A novel method for the determination of organophosphate pesticide residues in ham at the same time was established. [Method] Organophosphate pesticide residues in ham were extracted by acetonitrile， the liquid-liquid extraction using acetonitrile and n-hexane as the extraction volvent was used to remove the grease and pigment and then， the solution was purified by carbon solid phase extraction column， detected by the flame photometry detector of gas chromatograph. [Result] Experimental results showed that 16 species of organophosphate pesticides were well separated in DB-17 and DB-1. Within the scope of 0.05 to 1.00 μg/mL， pesticide residues chromatography analysis of the linear relationship was good to meet quantitative analysis requirements. The average recoveries of organic phosphorus pesticides were 7196%-117.21%， spiked at 0.08 and 0.20 mg/kg level. The relative standard deviations for all the compounds were 1.73%-12.84%. The detection limit of the method varied between 0.005 3-0.011 8 mg/kg. [Conclusion] The method is simple， precise， sensitive， and has a good separation effect， it can be applied to the routine analysis for organophosphate pesticide residues in ham.

Key words Ham；Liquid-liquid extraction；Solid-phase extraction；Gas chromatography；Organophosphate pesticide

火腿即腌制或熏制的豬肉，味美且營養豐富，歷來被看作是席上佳肴、饋贈珍品，深受國人喜愛，每年消費數萬噸。然而，一些不法廠商為了避免蚊蟲叮咬和生蛆等問題，在制作過程中添加了劇毒農藥，給火腿質量安全帶來了極大隱患，嚴重威脅著消費者的身體健康。因此，建立一種快速、準確地測量火腿中農藥殘留量的分析方法對有效解決其質量安全問題具有重要意義。目前，檢測有機磷農藥的方法主要有分光光度法[1]、傳感器法[2]、流動注射法[3]、氣相色譜法[4-5]、液相色譜法[6]、氣質聯用法[7]、液質聯用法[8]等，但對于火腿中有機磷農藥殘留量的報道還較少。其中部分方法[9]需要用到氣質聯用儀、凝膠滲透色譜等大型、高精密度儀器，成本較昂貴；……