Zhang Wen-Hua, Xie Wen, Hou Jian-Bo, Hu Xiao-Li, Wang Peng, Zhang Ya-Qin, Xu Dun-Ming
Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou, P.R. China.
Technic Center of Xiamen Customs, Xiamen, P.R. China.
J Sep Sci. 2021 Sep;44(18):3516-3523. doi: 10.1002/jssc.202100303. Epub 2021 Jul 8.
In this paper, a method for the separation of triadimenol stereoisomers using ultra-performance convergence chromatography and an analytical method for the determination of triadimenol stereoisomer residues in pumpkin puree, apple puree, and tomato puree as a supplement for infants are established. Test samples were extracted with acetonitrile and successively purified with graphitized carbon black and Florisil column. Afterward, Acquity Trefoil AMY1 column was adopted for chiral separation of chromatographic column, and gradient elute was carried out with supercritical carbon dioxide-methanol as the mobile phase and with external standard method for quantitation. Results showed that the linearly dependent coefficient of the four kinds of triadimenol stereoisomers within 1.0 and 50 mg/L was greater than 0.9997, and the limit of quantitation of the four kinds of triadimenol stereoisomers was 0.05 mg/kg. Recovery experiment was carried out within 0.05 and 1.0 mg/kg scope, the recoveries were 81.0-107％, and the relative standard deviation was 2.3-7.6%. This method implemented the separation of triadimenol stereoisomers and its residue test in pumpkin puree, apple puree, and tomato puree as a supplement for infants, and it can provide reliable technical support for the analysis of pesticide residue and assessment of product quality.
本文建立了一种采用超高效收敛色谱法分离三唑醇立体异构体的方法，以及一种测定南瓜泥、苹果泥和番茄泥中三唑醇立体异构体残留量作为婴儿辅食的分析方法。测试样品用乙腈提取，依次经石墨化炭黑和弗罗里硅土柱净化。之后，采用Acquity Trefoil AMY1手性分离色谱柱，以超临界二氧化碳 - 甲醇为流动相进行梯度洗脱，外标法进行定量。结果表明，4种三唑醇立体异构体在1.0～50mg/L范围内线性相关系数大于0.9997，4种三唑醇立体异构体的定量限为0.05mg/kg。在0.05～1.0mg/kg范围内进行回收率实验，回收率为81.0%～107%，相对标准偏差为2.3%～7.6%。该方法实现了三唑醇立体异构体的分离及其在南瓜泥、苹果泥和番茄泥婴儿辅食中的残留检测，可为农药残留分析和产品质量评估提供可靠的技术支持。
