超高效液相色谱-四极杆串联离子阱复合质谱法同时测定药食同源中药材中6种玉米赤霉醇类真菌毒素

Simultaneous determination of 6 kinds of zearalenol mycotoxins in Chinese medicinal materials homologous to medicine and food by ultra performance liquid chromatography-quadrupole ion trap mass spectrometry

中文关键词:  药食同源中药材  玉米赤霉醇类真菌毒素  超高效液相色谱-四极杆串联离子阱复合质谱法

英文关键词:Chinese medicinal materials homologous to medicine and food  zearalenol mycotoxins  ultra performance liquid chromatography-quadrupole ion trap mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-四极杆串联离子阱复合质谱法同时测定药食同源中药材中6种玉米赤霉醇类真菌毒素的分析方法。方法 样品经乙腈-甲酸-水(80:1:19, V:V:V)提取, MLJ-1多重基质吸附型固相萃取柱净化, Waters BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 流动相为乙腈和0.1%甲酸水溶液梯度洗脱, 电喷雾负离子模式电离, 质谱扫描模式为多反应监测-信息关联扫描-增强子离子(multiple response monitoring-information dependent acquisition-enhanced product ion, MRM-IDA-EPI), 外标法定量。结果 6种玉米赤霉醇类真菌毒素在0.1~20.0 ng/mL范围内线性关系良好, 相关系数(r)均大于0.994, 平均加标回收率为83.4%~99.7%, 相对标准偏差为2.7%~7.4%, 6种真菌毒素检出限为0.3~0.5 μg/kg。结论 本方法应用超高效液相色谱-四极杆串联离子阱复合质谱法特有的MRM-IDA-EPI扫描模式, 可同时实现6种玉米赤霉醇类真菌毒素的准确定性、定量分析及可疑峰筛查、确证。

英文摘要:

      Objective To establish a method for the simultaneous determination of 6 kinds of zearalenol mycotoxins in Chinese medicinal materials homologous to medicine and food by ultra high performance liquid chromatography quadrupole tandem ion trap composite mass spectrometry. Methods The samples were extracted with acetonitrile and formic acid and water (80:1:19, V:V:V), purified by MLJ-1 purification of solid phase extraction column with multiple matrix adsorption, and separated with C18 chromatographic column (100 mm×2.1 mm, 1.7 μm) for gradient elution using acetonitrile and 0.1% formic acid aqueous solution as mobile phase, ionized by electrospray negative ion mode, detected by multiple response monitoring-information dependent acquisition-enhanced product ion (MRM-IDA-EPI) mass spectrum scanning mode and quantified by external standard method. Results The linear relationships of 6 kinds of zearalenol mycotoxins were good in the range of 0.1-20.0 ng/mL, and the correlation coefficients (r) were greater than 0.994. The average recoveries were 83.4%?99.7%, the relative standard deviations were 2.7%?7.4%, and the detection limits of 6 kinds of mycotoxins were 0.3?0.5 μg/kg. Conclusion The MRM-IDA-EPI scanning mode of ultra performance liquid chromatography-quadrupole tandem ion trap composite mass spectrometry is used to realize the accurate qualitative and quantitative analysis of 6 kinds of zearalenol mycotoxins and the screening and confirmation of suspicious peaks.