| 血清和尿液中22种真菌毒素的高效液相色谱——四极杆轨道阱质谱筛查方法建立 |
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| 引用本文： | 陈佳玥,' target='_blank'>,李卓雅,黄鑫仪,任建伟,俞凌云,骆春迎,张静,蒋建军,邹晓莉.血清和尿液中22种真菌毒素的高效液相色谱——四极杆轨道阱质谱筛查方法建立[J].现代预防医学,2022,0(6):1109-1117. |
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| 作者姓名： | 陈佳玥 ' target='_blank'> 李卓雅 黄鑫仪 任建伟 俞凌云 骆春迎 张静 蒋建军 邹晓莉 |
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| 作者单位： | 1.四川大学华西公共卫生学院/四川大学华西第四医院，四川 成都 610041；2.成都市疾病预防控制中心；3.成都海关技术中心，四川 成都 610041 |
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| 摘 要： | 目的 建立血液、尿液中22种常见真菌毒素的液液萃取-高效液相色谱四极杆轨道阱质谱测定方法。方法 基于高效液相色谱-四极杆轨道阱质谱技术，首先建立22种常见真菌毒素的色谱质谱数据库。然后取血清和尿液样品，用0.10 mol/L NaOH 溶液调节至碱性，加入乙酸乙酯涡旋混合萃取，萃取液用弱的氮气吹至近干，残渣加甲醇水溶液（50∶50,v/v）复溶，经过滤后进 LC - MS/MS 分析。在一定识别标准下与数据库比对进行定性筛查。结果 尿液和血液检出限（limit of detection，LOD）分别为2.61×10 - 3～50.0 ng/ml和2.07×10 - 3～50.0 ng/ml，定量限（limit of quantitation，LOQ）分别为8.70×10 - 3～1.67×102 ng/ml和 6.91×10 - 3～1.67×102 ng/ml。尿液测定日内相对标准偏差（relative standard derivations, RSDs）为2.34%～8.40%，日间RSDs为4.80%～10.9%；血液测定日内RSDs为2.10%～10.6%，日间RSDs为3.07%～11.6%。结论 建立的快速筛查方法操作简单，具有高通量、高灵敏度和高准确性的特点，符合生物样品中毒物分析鉴定的要求，同时可以更好地发现新型毒物和未知毒物。
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| 关 键 词： | 真菌毒素 血液 尿液 液相色谱 - 四极杆轨道阱质谱法 |
Establishment of a screening method for 22 mycotoxins in blood and urine by high performance liquid chromatography-quadrupole tandem orbitrap mass spectrometry |
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| CHEN Jia-yue,LI Zhuo-ya,HUANG Xin-yi,REN Jian-wei,YU Ling-yun,LUO Chun-ying,ZHANG Jing,JIANG Jian-jun,ZOU Xiao-li.Establishment of a screening method for 22 mycotoxins in blood and urine by high performance liquid chromatography-quadrupole tandem orbitrap mass spectrometry[J].Modern Preventive Medicine,2022,0(6):1109-1117. |
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| Authors: | CHEN Jia-yue LI Zhuo-ya HUANG Xin-yi REN Jian-wei YU Ling-yun LUO Chun-ying ZHANG Jing JIANG Jian-jun ZOU Xiao-li |
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| Affiliation: | *West China School of Public Health and West China Fourth Hospital, Sichuan University, Chengdu, Sichuan 610041, China |
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| Abstract: | Objective To establish the method of screening 22 kinds of common mycotoxins in blood and urine by high performance liquid chromatography-quadrupole tandem orbitrap mass spectrometry (HPLC-Q-orbitrap MS). Methods Firstly, based on HPLCQ-orbitrap MS, the database of chromatography-mass spectrometry for 22 kinds of common mycotoxins was established for the screening and identification. After the pH value being adjusted to alkalinity with 0.10 mol/L NaOH solution, ethyl acetate was added to extract the target analytes by vortex mixing. Then the extractant was collected and dried-up under gentle nitrogen flow, and the residue was redissolved with methanol-water (50:50, v/v) and filtrated with a 0.22 μm filter. Finally, the filtrate was used for LC-MS/MS analysis. The results were analyzed and compared with the database for qualitative screening under certain identification standards. Results The method detection limits (MDLs) for the urine and blood sample were 2.61×10-3 to 50.0 ng/ml and 2.07×10-3 to 50.0 ng/ml, respectively. The method quantitative limits (MQLs) for the urine and blood sample were 8.70×10-3 to 1.67×102 ng/ml and 6.91×10-3 to 1.67×102 ng/ml, respectively. The intra-day RSDs of urine samples were 2.34%-8.40% and the inter-day RSDs were 4.80%-10.9%. The intra-day RSDs of blood samples were 2.10%-10.6%, and the inter-day RSDs were 3.07%-11.6%. Conclusion The proposed method is simple to operate, has the characteristics of high throughput, high sensitivity and high accuracy, which can meet the requirements of poison identification in biological samples, and can better identify new and unknown poisons. |
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| Keywords: | Mycotoxins Blood Urine HPLC-Q-orbitrap MS |
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