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| 高效液相色谱法定量检测牛奶中八氯苯乙烯残留量 |
| Determination of octachlorostyrene residues in milk by high performance liquid chromatography |
| 投稿时间：2025-03-07 修订日期：2025-04-29 |
| DOI： |
| 中文关键词: 牛奶 八氯苯乙烯 残留量 高效液相色谱法 |
| 英文关键词:milk octachlorostyrene residue high performance liquid chromatography |
| 基金项目:山东农业工程学院博士科研基金(项目编号:BSQJ201808) |
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| 中文摘要: |
| 目的 建立高效液相色谱法检测牛奶中八氯苯乙烯残留量检测的分析方法。方法 牛奶中的八氯苯乙烯经乙腈提取，用氯化钠和无水硫酸镁除脂，提取液离心、过微孔滤膜后上机分析，采用Waters C18色谱柱(250 mm×4.6 mm，5μm)分离，以0.3%的三氟乙酸溶液（pH=3.2）-乙腈(20:80，V/V)为流动相进行等度洗脱，紫外检测器检测，外标法定量。结果 八氯苯乙烯在0.1～2.0 ng/mL的标准质量浓度范围内线性关系良好，相关系数r大于0.999。样品中八氯苯乙烯的检出限为0.05 μg/kg，定量限为0.1 μg /kg。在0.1～0.4 μg/kg添加浓度范围内，八氯苯乙烯的回收率均为70%～90%，相对标准偏差均小于10%。结论 该方法具有简便快捷、灵敏度高和定性准确等特点，适用于牛奶中八氯苯乙烯残留量的检测，为政府的食品、农产品质量监管工作提供有效的技术支撑。 |
| 英文摘要: |
| Objective High performance liquid chromatography (HPLC) method by the established and optimized conditions for the determination of octachlorostyrene residues in milk. Methods Milk samples were extracted with acetonitrile and cleared up by sodium chloride and anhydrous magnesium sulfate, filtered through a microporous membrane, and analyzed by the high performance liquid chromatography. The separation was performed on a Waters C18 column (250 mm×4.6 mm, 5 μm) with gradient elution by using 0.3% trifluoroacetic acid solution（pH=3.2） and acetonitrile(20:80，V/V) as the mobile phase, and quantified by external standard method. Results The results indicated that the correlations were greater than 0.999 at the range of 0.1 to 2.0 ng/mL . The limit of detection of octachlorostyrene was 0.05 μg/kg,and the limit of quantification was 0.1 μg/kg. The average recoveries of octachlorostyrene ranged from 70% to 90% at spiled levels of 0.1 to 0.4 μg/kg with RSD less then 10%. Conclusion The experiment show that the method is simple, rapid, high sensitivity, good reproducibility and suitable for detection of octachlorostyrene residues in milk .The method provide effective technical support to the government's food and agricultural product quality supervision work. |
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