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

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DOI 10.19812/j.cnki.jfsq11-5956/ts.20250307003
刊名
Journal of Food Safety and Quality
年,卷(期) 2025, 16(12)
作者
作者单位

山东农业工程学院食品科学与工程学院;
山东省畜产品质量安全中心

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, 5 μm)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0.10 μg /kg。在0.10~0.40 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。
Abstract
Objective To establish and optimize conditions for the determination of octachlorostyrene residues in milk by high performance liquid chromatography (HPLC) method. 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 quantitation 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 relative standard deviation 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.
关键词
牛奶;八氯苯乙烯;残留量;高效液相色谱法
KeyWord
milk; octachlorostyrene; residue; high performance liquid chromatography
基金项目
页码 140-144
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李淑焕, 张雨桐, 张兆雪, 张呈军, 赵丰华, 刘霄飞, 李玉姣, 薄永恒*. 高效液相色谱法定量检测牛奶中八氯苯乙烯残留量 [J]. 食品安全质量检测学报. 2025; 16; (12). 140 - 144.

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