QuEChERS-液相色谱-串联质谱法测定果蔬及其制品中噻霉酮残留
投稿时间：2015-09-04      点此下载全文 HTML
引用本文：粟有志,周均,孟茹,等.QuEChERS-液相色谱-串联质谱法测定果蔬及其制品中噻霉酮残留[J].农药学学报,2016,18(1):135-140.
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作者单位E-mail
粟有志 伊犁出入境检验检疫局综合技术服务中心, 新疆伊宁 835000 suyouzhi1110@163.com 
周均 伊犁出入境检验检疫局综合技术服务中心, 新疆伊宁 835000  
孟茹 伊犁出入境检验检疫局综合技术服务中心, 新疆伊宁 835000  
李娜 伊犁师范学院化学与生物科学学院, 新疆伊宁 835000  
李艳美 伊犁出入境检验检疫局综合技术服务中心, 新疆伊宁 835000  
罗琼 伊犁出入境检验检疫局综合技术服务中心, 新疆伊宁 835000  
基金项目:新疆维吾尔自治区自然科学基金资助项目(201442137-23).
中文摘要:建立了QuEChERS-液相色谱-串联质谱(HPLC-MS/MS)测定果蔬及其制品中噻霉酮的分析方法。样品经含0.1%乙酸的乙腈提取,聚苯乙烯/二乙烯苯(PEP)和C18粉净化,以0.1%甲酸水溶液(含2 mmol/mL乙酸铵)和甲醇为流动相梯度洗脱,经C18色谱柱分离,正离子模式扫描,多重反应监测模式检测。以保留时间和特征离子对(母离子和两个碎片离子)信息比较进行定性,基质匹配外标法定量。结果表明:在10~500 ng/mL范围内,噻霉酮在黄瓜、葡萄、葡萄干、番茄酱、番茄和苹果6种基质中的决定系数(R2)均大于0.996;定量限(LOQ) (以S/N≥10计)为10.0 μg/kg,在10、20和100 μg/kg 3个添加水平下,平均回收率在80%~98%,相对标准偏差(RSD)在2.4%~13%。该方法高效快捷、准确度和精密度均符合农药残留检测要求。
中文关键词:QuEChERS  液相色谱-串联质谱  果蔬及其制品  噻霉酮  残留
 
Determination of benziothiazolinone residue in vegetable and fruit by QuEChERS-liquid chromatography-tandem mass spectrometry
Abstract:A method for the determination of benziothiazolinone in vegetable and fruit was developed using QuEChERS-liquid chromatography-tandem mass spectrometry. The sample was extracted with acidic acetonitrile, and then cleaned up by PEP and C18. The analyte was separated on C18 column by gradient elution with methanol-0.1% formic acid in water (including 2 mmol/mL ammonium acetate) as the mobile phases. Benziothiazolinone was determined by electrospray positive ion source (ESI+), and multiple reaction monitoring mode (MRM). The qualitative analysis was based on the retention times and characteristic ion pairs consisting of one parent ion and two fragment ions, and the quantitative analysis was carried out by the matrix-matched external standard method. The results showed that calibration curves had good linearity for benziothiazolinone and the determination coefficients (R2) were larger than 0.996; the limits of quantification (LOQs, S/N≥10) of benziothiazolinone in six different matrix (cucumber, grape, raisin, tomato sauce, tomato, apple) were10.0 μg/kg. At spiked three levels of 10, 20, 100 μg/kg in negative samples, the recoveries of benziothiazolinone were in the range of 80%-98% and the RSDs were in the range of 2.4%-13%. This novel method is highly effective, and the sensitivity, accuracy and precision are suitable for the monitoring of pesticide residues.
Key words:QuEChERS  liquid chromatography-tandem mass spectrometry (HPLC-MS/MS)  vegetable and fruit foods  benziothiazolinone  residue
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