|
| QuEChERS净化结合超高效液相色谱-串联质谱法快速检测汉中面皮中米酵菌酸含量 |
| Determination of bongkrekic acid content in Hanzhong Mianpi by QuEChERS purification combined with ultra-high performance liquid chromatography-tandem mass spectrometry |
| 投稿时间：2024-12-16 修订日期：2025-05-09 |
| DOI： |
| 中文关键词: 超高效液相色谱-串联质谱法 QuEChERS净化 米酵菌酸 汉中面皮 |
| 英文关键词:ultra-high performance liquid chromatography-tandem mass spectrometry QuEChERS purification bongkrekic acid Hanzhong Mianpi |
| 基金项目:陕西省市场监督管理局2022 年度科技计划项目：汉中面皮中椰毒假单胞菌酵米面亚种及 其毒素的污染调查与风险控制（2022KY27） |
|
|
|
|
| 摘要点击次数: 3 |
| 全文下载次数: 0 |
| 中文摘要: |
| 目的 建立一种QuEChERS前处理净化结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速检测汉中面皮中米酵菌酸含量的方法。方法 面皮样品采用乙腈-水(8:2, V:V)超声提取，QuEChERS净化处理，浓缩、定容，选用Thermo (100 mm×2.1 mm，1.8 μm)色谱柱分离，以乙腈和(0.1%)甲酸水溶液进行梯度洗脱，电喷雾离子源(electron spray ionization, ESI)，负离子多反应监测(multiple reaction monitoring, MRM)模式，以标准曲线法定量。结果 米酵菌酸在1~100 μg/Lng/mL范围内线性关系良好，相关系数(r2)大于0.999，在2、10、50 μg/kg低中高3个加标水平下，加标回收率为86.7%~90.0%，相对标准偏差(relative standard deviation, RSD)为2.3%~2.9%，方法检出限为0.5 μg/kg，定量限为1.5 μg/kg。所有样品均未检出米酵菌酸。结论 该方法前处理简单、分析快速、回收率高、灵敏度高，可为汉中面皮中米酵菌酸的质量控制提供参考。 |
| 英文摘要: |
| Objective To establish a method for rapid determination of bongkrekic acid content in Hanzhong Mianpi by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) combined with QuEChERS purification. Methods The Hanzhong Mianpi samples were extracted by acetonitrile water (8:2, V:V) ultrasoundnic extraction, purified by QuEChERS, concentrated, and made toconstant volume, and then separated usingby Thermo (100 mm×2.1 mm, 1.8 μm) chromatographic column. The mobile phase was acetonitrile (A). 0.1% formic acid solution (B) using a gradient elution method. The bongkrekic acid was detected in eletron spray ionization with negative ion mode (ESI-) with multi-reaction monitoring (MRM). The contents were calculated using the standard curve method. Results The correlation coefficient (r2) of bongkrekic acid was not less than 0.999 in the range of 1-100 μg/Lng/mL. The recoveries were 86.7%-90.0% at 2, 10, 50 μg/kg levels respectively, relative standard deviation (RSD) was 2.3%-2.9%. The limit of detection of the method was 0.5 μg/kg, the limit of quantitative was 1.5 μg/kg. No bongkrekic acid were detected in all samples. Conclusion This method has simple pre-treatment, fast analysis, high recovery rate, and high sensitivity, which can provide reference for the quality control of bongkrekic acid in Hanzhong Mianpi. |
| 查看全文 查看/发表评论 下载PDF阅读器 |
| 关闭 |
