摘要
[目的]建立QuEChERS-液相色谱-串联质谱法测定植物源农产品中丁硫克百威残留量的分析方法。[方法]优化仪器条件、样品提取条件和净化条件中无水MgSO4用量,通过液相色谱-串联质谱仪测定,同时采用基质匹配标准系列溶液进行校准,外标法定量。[结果]流动相采用甲醇-水。对于蔬菜、水果、食用菌,采用10 mL乙腈提取,4 g无水MgSO4和2 g NaOAc为提取盐包;对于茶叶和粮谷类,采用15 mL乙腈提取,6 g无水MgSO_(4)和3 g NaOAc为提取盐包。净化方式采用QuEChERS技术,且无水MgSO4用量均为720 mg。本方法各基质中丁硫克百威的检出限为0.064~0.46μg/kg,定量限为1~5μg/kg。各种基质在各自线性范围内线性关系均良好(r>0.990),在添加质量分数1~50μg/kg范围内,各基质中的回收率介于73.09%~113.72%之间,相对标准偏差RSD(n=6)在2.10%~9.26%之间,且除萝卜基质外,处理后的样液在24 h内稳定。[结论]方法灵敏度高,回收率和精密度均较好,且操作简便、高效、对仪器污染少、节约成本,适用于对植物源农产品中丁硫克百威残留量进行定性和定量检测。
[Aims]To establish an analytical method for the determination of carbosulfan residues in plant-based agricultural products by QuEChERS-liquid chromatography-tandem mass spectrometry(QuEChERS-LC-MS/MS).[Methods]The instrument conditions,sample extraction conditions and the dosage of anhydrous MgSO4 in purification conditions were optimized.The analysis was performed using LC-MS/MS,with quantification via the external standard method,employing matrix-matched standard series solutions for calibration.[Results]The mobile phase adopted methanol-water.For vegetables,fruits and edible fungi,10 mL of acetonitrile was used for extraction,4 g of anhydrous MgSO_(4) and 2 g of NaOAc were used as the extraction salt packets.For tea and grains,15 mL of acetonitrile was used for extraction,6 g of anhydrous MgSO4 and 3 g of NaOAc were used as the extraction salt packets.The QuEChERS technology was adopted as purification method,and the dosage of anhydrous MgSO4 was 720 mg for all.The detection limits of carbosulfan in matrices of this method were 0.064-0.46μg/kg,and the quantification limits were 1-5μg/kg.The linear relationships of all matrices were good within their respective linear ranges(r>0.990).Within the spiked mass fraction range of 1-50μg/kg,the recovery rates of each matrix ranged from 73.09%to 113.72%,and the RSD(n=6)ranged from 2.10%to 9.26%.Moreover,except for radish matrix,the processed samples were stable within 24 h.[Conclusions]This method exhibited high sensitivity,favorable recovery rate and precision,while offering easy operation,high efficiency,less contamination to the instrument,and cost savings.It is suitable for both qualitative and quantitative detection of carbosulfan residues in plant-based agricultural products.
作者
田甜
吴刚
高进
赵静
唐澈
陈华斌
余静
曾军
王伟
吴君哲
杨艳
TIAN Tian;WU Gang;GAO Jin;ZHAO Jing;TANG Che;CHEN Huabin;YU Jing;ZENG Jun;WANG Wei;WU Junzhe;YANG Yan(Hubei Agricultural Product Quality and Safety Testing Center/Inspection and Testing Center of Agricultural Products Quality and Safety,Ministry of Agriculture and Rural Affairs(Wuhan),Wuhan 430070,China)
出处
《农药》
北大核心
2025年第12期904-910,919,共8页
Agrochemicals
基金
湖北省农产品质检中心创新项目资助。
