HPLC Determination of Omethoate Content in Soil
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摘要: 采用高效液相色谱法优化了土壤中的氧化乐果残留测定条件，优化结果为：色谱柱为Inertsil QDS-SP 4.6*250 mm，流动相为甲醇/水（V/V=10/90），溶剂为超纯水，检测波长210 nm，柱温25℃，进样量为20 μL，总流速1.0 mL·min-1；氧化乐果在0.1～10.0 μg·mL-1范围内，其质量浓度与峰面积呈良好的线性关系（R2=0.9992），最低检测限0.1 μg·mL-1。采用振荡提取法，提取剂为丙酮和乙酸乙酯，提取后的溶液以弗罗里硅土为固相萃取柱，淋洗剂为丙酮/乙腈（1/3）。采用上述方法对土壤样品进行测定，加标回收率为在70%～120%，相对标准偏差在2.08%～8.08%，说明该方法的准确度和精密度均符合农药残留分析的要求，适合土壤中氧化乐果的残留量检测。Abstract: Testing conditions for the omethoate determination byHPLC were optimized to be: Inertsil QDS-SP (4.6*250 μm) at 25℃, an injection of 20μL methanol/water (V/V=10/90) as mobile phase ata flow rate of 1.0 mL·min-1, and the wave length of 210 nm for ultraviolet detection. A high recovery rate was achieved by using anextraction column with acetone/acetonitrile (V/V=1/3) as the eluting agent. A linear calibration curve for the omethoate concentrations in the range of 0.1-10μg·mL-1(R2=0.9992) with a minimal detection limit of 0.1 μg·mL-1 was established. Acetone and ethyl acetate were used as the solvents in the oscillation extraction. The recovery rate of omethoate in the soil samples ranged from 70% to 120% with a relative deviation of 2.08%-8.08%, which was within the requirements for pesticide residue analysis. It appeared that the newly developed HPLC methodology was appropriate for detecting omethoate residues in soil.
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Key words:
- HPLC /
- omethoate /
- soil /
- organophosphorus pesticides
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图 1 优化条件下氧化乐果的高效液相色谱
Figure 1. Chromatogram of Omethoate under optimized HPLC testing conditions
图 2 氧化乐果标准溶液与峰面积的关系
Figure 2. Correlation between omethoate standard solutions and peak areas under curve
表 1 不同层析柱和不同淋洗剂对氧化乐果回收率的比较
Table 1. Comparison of different columns and eluting agents on omethoate recovery rate
净化填料 标样含量/
(μg·mL-1)平均回收率/% 1 2 3 弗罗里硅土 1.0 31 41 99.85 中性氧化铝 1.0 - - - 注：1, 2, 3分别表示淋洗液丙酮和二氯甲烷(1:1)、丙酮和正己烷(3:1)、丙酮和乙腈(1:3)， 
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表 2 土壤样品测定的氧化乐果的重复性和回收率
Table 2. Data repeatability and recovery of omethoatein soil samples
组分 加标量/
(μg·g-1)单次加标回收率/% 平均加标回
收率/%RSD
/%1 2 3 4 5 6 梨园风沙土 0.075 91.2 94.3 94.5 100.4 93.2 94.8 94.83 4.17 0.150 86.9 85.3 83.6 85.4 87.5 86.4 85.85 2.03 0.750 75.5 75.5 80.9 73.0 75.2 76.8 76.15 4.41 莱阳褐土 0.075 100.2 110.2 119.8 106.5 116.1 111.0 110.65 8.08 0.150 95.6 97.4 98.9 100.5 98.2 99.2 98.3 2.08 0.750 94.5 90.1 89.2 93.6 87.8 92.4 91.28 3.59
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表 3 两种不同土壤的理化性质
Table 3. Physical and chemical properties of two sampled soils
pH 有机质 N P K CEC 梨园风沙土 6.43 6.86 43.96 53.25 130.83 120.13 莱阳褐土 7.28 12.36 36.63 17.44 125.83 31.06
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