| 朱筱玲1，赵淑娥1，罗春丽1，熊远珍2.超声辅助-分散液液微萃取/快速液相色谱-串联质谱法测定食用植物油中黄曲霉毒素[J].中国油脂,2019,44(11):97~101.[ZHU Xiaoling1, ZHAO Shue1, LUO Chunli1, XIONG Yuanzhen2.Determination of aflatoxins in edible oils by ultrasound-assisted-dispersive liquid-liquid microextraction(UA-DLLME) /RRLC-MS/MS[J].China Oils and Fats,2019,44(11):97~101.] |
| 超声辅助-分散液液微萃取/快速液相色谱-串联质谱法测定食用植物油中黄曲霉毒素 |
| Determination of aflatoxins in edible oils by ultrasound-assisted-dispersive liquid-liquid microextraction(UA-DLLME) /RRLC-MS/MS |
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| DOI：10.12166/j.zgyz.1003-7969/2019.11.019 |
| 中文关键词: 超声辅助-分散液液微萃取 快速液相色谱-串联质谱法 黄曲霉毒素 食用植物油 |
| 英文关键词:ultrasound-assisted-dispersive liquid-liquid microextraction RRLC-MS/MS aflatoxin edible oil |
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| 中文摘要: |
| 建立了超声辅助-分散液液微萃取(UA-DLLME)/快速液相色谱-串联质谱法（RRLC-MS/MS）测定食用植物油中黄曲霉毒素（AFB1、AFB2、AFG1、AFG2）的方法。先以分散剂溶解样品，再以萃取剂萃取，离心后底层溶液经脱脂上机，在电喷雾离子源正离子模式(ESI+)下采用多反应监测模式(MRM)监测。对样品前处理方法进行了优化。结果表明，最优样品前处理条件为：1 g样品，2 mL石油醚为分散剂，1 000 μL乙腈-水（体积比8∶ 2）为萃取剂，超声辅助萃取时间2 min，离心时间5 min，离心转速4 000 r/min。该方法的线性范围为0.625~30.0 ng/mL，相关系数均大于0.998，加标回收率为88.2%~101.5%，相对标准偏差均小于3.3%。该方法简便、快速、经济、准确度和精密度高且环境友好，适合食用植物油中黄曲霉毒素的定性和定量测定。 |
| 英文摘要: |
| A method of ultrasound-assisted-dispersive liquid-liquid microextraction(UA-DLLME) and rapid resolution liquid chromatography-tandem mass spectrometry （RRLC-MS/MS）was estabished to detect aflatoxins(AFB1, AFB2, AFG1, AFG2) in edible oils. The sample was dissolved in dispersing agent, extracted by extractant, then the bottom solution after centrifugation was defatted and injected into RRLC-MS/MS. Target aflatoxins were analyzed in positive electrospray ionization(ESI+) under multiple reaction monitoring(MRM) mode. The sample pretreatment method was optimized. The results showed that the optimal pretreatment conditions were obtained as follows: 1 g sample, 2 mL petroleum ether as dispersing agent, 1 000 μL acetonitrile-water(volume ratio 8∶ 2) as extractant, UA extraction time 2 min, centrifugation time 5 min, centrifugation speed 4 000 r/min. The linearity of the established method was in the range of 0.625-30.0 ng/mL, the correlation coefficients were above 0.998, the recoveries of spiked samples were in the range of 88.2%-101.5% and the relative standard deviations were less than 3.3%.The method had items of simpleness, rapidness, low cost, high accuracy and precision, environmental friendliness and was suitable for qualitative and quantitative analysis of aflatoxins in edible oils. |
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