| 何京明,苏丽梅,石梁稳,唐标,韦东,李治尧,黄梅贵,刘守廷,班燕宁.固相萃取/液相色谱-串联质谱法测定沃柑中春雷霉素、双胍辛烷基磺酸盐的残留量[J].中国南方果树,2024,53(5): |
| 固相萃取/液相色谱-串联质谱法测定沃柑中春雷霉素、双胍辛烷基磺酸盐的残留量 |
| Residue Content Analysis of Kasugamycin and Iminoctadine Tris in Orah Using Solid-Phase Extraction/Liquid Chromatography-Tandem Mass Spectrometry. |
| 投稿时间：2023-10-17 修订日期：2023-12-29 |
| DOI： |
| 中文关键词: 沃柑 液相色谱-质谱 春雷霉素 双胍辛烷基磺酸盐(双胍辛胺) |
| 英文关键词:Orah Liquid Chromatography-Tandem Mass Spectrometry Kasugamycin Iminoctadine Tris(Iminoctadine) |
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| 中文摘要: |
| 采用高效液相色谱-质谱联用技术(HPLC-MS/MS)同时提取同时测定了沃柑中春雷霉素、双胍辛烷基磺酸盐两种极性杀菌剂农药。用0.2%甲酸水溶液提取,采用HLB先净化,再分别经SCX强阳离子交换固相萃取柱和WCX弱阳离子交换固相萃取柱除沃柑中的干扰物质,然后用C18-AQ高效液相色谱柱在正电喷雾模式下进行多重反应监测(MRM)分析,以基质匹配标准曲线外标法定量。杀菌剂春雷霉素、双胍辛胺浓度与峰面积呈良好的线性关系,在0.5μg/mL ~ 200 μg/mL范围内线性相关系数为0.9996。该方法灵敏度高,色谱性能优良。结果表明,该方法春雷霉素、双胍辛烷基磺酸盐的加标回收率分别为67.88%~93.5%和62.64%~84.36%。沃柑中春雷霉素、双胍辛胺的定量检出限(LOQ)均为0.0004 mg/kg,通过3家实验室比对,其结果的相对标准偏差分别为9.89%和9.75%,重复性好。 |
| 英文摘要: |
| The simultaneous extraction and determination of two polar fungicides, Kasugamycin and Iminoctadine Tris in Orah were carried out using High-Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS) technology. The extraction was performed with a 0.2% formic acid aqueous solution. After purification using HLB, interference substances in the oranges were further eliminated by Solid-Phase Extraction columns with strong cation-exchange (SCX) and weak cation-exchange (WCX) resins. Subsequently, the analysis was conducted by Multiple Reaction Monitoring (MRM) in positive electrospray ionization mode using a C18-AQ high-performance liquid chromatography column, and quantification was performed using an external standard calibration curve. Kasugamycin and Iminoctadine Tris showed a good linear relationship between concentration and peak area in the range of 0.5 μg/mL to 200 μg/mL, with a linear correlation coefficient of 0.9996. The method demonstrated high sensitivity and excellent chromatographic performance. The results indicated that the spiking recoveries of Kasugamycin and Iminoctadine Tris were in the range of 67.88% to 93.5% and 62.64% to 84.36%, respectively. The limits of quantification (LOQ) for Kasugamycin and Iminoctadine in Orah were both 0.0004 mg/kg. Interlaboratory comparisons involving three labs showed relative standard deviations (RSD) of 9.89% and 9.75%, indicating good repeatability. |
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