CAJ | 학술논문

传统的农药残留检测为理化检验方法，具有前处理过程繁琐、耗时、复杂等不足，以目前农业上使用较广的毒死蜱作为研究对象，提出了一种有机磷农药残留快速定量检测方法。首先，根据毒死蜱的化学特性，综合考虑比色剂的显色效果以及二次污染问题，确定在弱碱性环境下以间苯二酚对毒死蜱进行显色反应的预处理方案；然后，通过分析0.5～400 mg · kg -1之间毒死蜱样品的紫外-可见光光谱数据，确定了显色反应后的特征信息主要集中在365～420 nm之间。接着，以偏最小二乘法构建全谱预测模型，其校正相关系数达到0.9996，预测相关系数达到0.9956，校正标准差RMSEC为2.8147 mg · kg -1，验证标准差RM-SEP为8.0124 mg · kg -1；提取400 nm为中心波段的特征区域构建预测模型，其校正相关系数达到0.9996，预测相关系数达到0.9993，校正标准差RMSEC为2.6546 mg · kg -1，验证标准差RMSEP为3.4655 mg · kg -1。最后，通过分析0.5～16 mg · kg -1之间毒死蜱样品的近红外光谱数据，发现其显色功能团的特征不是很明显，但会引起间苯二酚本身5200 cm -1处吸收峰的变化。实验结果证明了所提出用于快速定量预测有机磷农药残留的方法是有效可行的，该方法通过比色剂的显色加强有机磷农药在全光谱特别是紫外-可见光范围内的信息，为实现农产品农药残留的快速检测提供了一条新途经。
전통적농약잔류검측위이화검험방법，구유전처리과정번쇄、모시、복잡등불족，이목전농업상사용교엄적독사비작위연구대상，제출료일충유궤린농약잔류쾌속정량검측방법。수선，근거독사비적화학특성，종합고필비색제적현색효과이급이차오염문제，학정재약감성배경하이간분이분대독사비진행현색반응적예처리방안；연후，통과분석0.5～400 mg · kg -1지간독사비양품적자외-가견광광보수거，학정료현색반응후적특정신식주요집중재365～420 nm지간。접착，이편최소이승법구건전보예측모형，기교정상관계수체도0.9996，예측상관계수체도0.9956，교정표준차RMSEC위2.8147 mg · kg -1，험증표준차RM-SEP위8.0124 mg · kg -1；제취400 nm위중심파단적특정구역구건예측모형，기교정상관계수체도0.9996，예측상관계수체도0.9993，교정표준차RMSEC위2.6546 mg · kg -1，험증표준차RMSEP위3.4655 mg · kg -1。최후，통과분석0.5～16 mg · kg -1지간독사비양품적근홍외광보수거，발현기현색공능단적특정불시흔명현，단회인기간분이분본신5200 cm -1처흡수봉적변화。실험결과증명료소제출용우쾌속정량예측유궤린농약잔류적방법시유효가행적，해방법통과비색제적현색가강유궤린농약재전광보특별시자외-가견광범위내적신식，위실현농산품농약잔류적쾌속검측제공료일조신도경。
The methods of physical-chemical inspection is adopted in the traditional pesticide residue detection ,which require a lot of pretreatment processes ,are time-consuming and complicated .In the present study ,the authors take chlorpyrifos applied widely in the present agricultural field as the research object and propose a rapid and quantitative detection method for organo-phosphorus pesticide residues .At first ,according to the chemical characteristics of chlorpyrifos and comprehensive chromogenic effect of several colorimetric reagents and secondary pollution ,the pretreatment of the scheme of chromogenic reaction of chlor-pyrifos with resorcin in a weak alkaline environment was determined .Secondly ,by analyzing Uv-Vis spectrum data of chlorpyri-fos samples whose content were between 0.5 and 400 mg · kg -1 ,it was confirmed that the characteristic information after the color reaction mainly was concentrated among 360~400 nm .Thirdly ,the full spectrum forecasting model was established based on the partial least squares ,whose correlation coefficient of calibration was 0.999 6 ,correlation coefficient of prediction reached 0.995 6 ,standard deviation of calibration (RMSEC) was 2.814 7 mg · kg -1 ,and standard deviation of verification (RMSEP) was 8.012 4 mg · kg -1 .Fourthly ,the wavelengths whose center wavelength is 400 nm was extracted as characteristic region to build a forecasting model ,whose correlation coefficient of calibration was 0.999 6 ,correlation coefficient of prediction reached 0.999 3 ,standard deviation of calibration (RMSEC) was 2.566 7 mg · kg -1 ,standard deviation of verification (RMSEP) was 4.886 6 mg · kg -1 ,respectively .At last ,by analyzing the near infrared spectrum data of chlorpyrifos samples with contents be-tween 0.5 and 16 mg · kg -1 ,the authors found that although the characteristics of the chromogenic functional group are not ob-vious ,the change of absorption peaks of resorcin itself in the neighborhood of 5 200 cm -1 happens .The above-mentioned experi-mental results show that the proposed method is effective and feasible for rapid and quantitative detection prediction for organo-phosphorus pesticide residues .In the method ,the information in full spectrum especially UV-Vis spectrum is strengthened by chromogenic reaction of a colorimetric reagent ,which provides a new way of rapid detection of pesticide residues for agricultural products in the future .