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微囊藻毒素的液-質(zhì)譜聯(lián)用和直接進(jìn)樣檢測(cè)方法比較

發(fā)布時(shí)間：2019/11/4 15:42:02     瀏覽次數(shù)：1002

微囊藻毒素的液-質(zhì)譜聯(lián)用和直接進(jìn)樣檢測(cè)方法比較
Comparison of Liquid Chromatography Tandem Mass Spectrometry and Direct Injection Methods for the Analysis of Microcystins
  
DOI：
中文關(guān)鍵詞: 微囊藻毒素  液-質(zhì)譜聯(lián)用  直接進(jìn)樣  螺螄

英文關(guān)鍵詞: Microcystin  liquid chromatography tandem mass spectrometry  direct injection analysis  Melanioides

采用高效液相色譜-串聯(lián)質(zhì)譜（LC-MS/MS）技術(shù)和直接進(jìn)樣（DIA）技術(shù)對(duì)7種微囊藻毒素進(jìn)行定性、定量分析，比較兩種方法在精密度、靈敏度、經(jīng)濟(jì)性等方面的優(yōu)缺點(diǎn)，并用于螺螄中微囊藻毒素的檢測(cè)。LC-MS/MS技術(shù)選用Waters XSelect HSS T3（2.1 mm × 150 mm，3.5 μm），用0.1%甲酸水溶液-0.1%甲酸乙腈溶液作流動(dòng)相，在電噴霧離子源（ESI）正離子多反應(yīng)離子檢測(cè)模式（MRM）下掃描，線性范圍為0.9965~0.9993，相對(duì)標(biāo)準(zhǔn)偏差3.6%~6.1%，檢出限和定量限分別小于0.54 ng/mL和1.81 ng/mL，回收率介于73.9%~83.4%之間。DIA技術(shù)選用碎片m/z 135.2為特征母核，優(yōu)化選定DP 60 eV和CE 55 eV，經(jīng)母離子掃描（PreIS）得到各微囊藻毒素的離子峰較為純凈，均以[M+2H]2+為主。兩種方法比較結(jié)果顯示：LC-MS/MS各項(xiàng)參數(shù)均優(yōu)于DIA，而DIA檢測(cè)速度較快，僅需1 min即可完成7種微囊藻毒素的快速測(cè)定。應(yīng)用兩種方法對(duì)60個(gè)隨機(jī)樣品的檢測(cè)表明，螺螄中的微囊藻毒素陽(yáng)性率達(dá)到63.3%，主要污染種類為MC-RR和LR。根據(jù)研究結(jié)果建議當(dāng)待測(cè)樣品數(shù)量較多時(shí)，首先采用DIA進(jìn)行初次篩選，對(duì)于陽(yáng)性樣品利用LC-MS/MS進(jìn)行二次檢測(cè)，可有效減少檢測(cè)時(shí)間、色譜柱損耗及溶劑消耗，提高結(jié)果的可靠性。本分析策略可用于快速分析水體及動(dòng)植物中的微囊藻毒素殘留，確定監(jiān)測(cè)物種、采樣站位和頻率、警戒值和防控反應(yīng)機(jī)制等，為相關(guān)部門完善和強(qiáng)化水產(chǎn)品監(jiān)測(cè)和管理工作提供科學(xué)依據(jù)，從而保障食用安全和近岸養(yǎng)殖業(yè)的健康發(fā)展。

 Seven molecular species of microcystins were qualitatively and quantitatively analyzed by both high performance liquid chromatography-tandem mass spectrometry （LC-MS/MS） and direct injection analysis （DIA）. The advantages and disadvantages of these two methods in precision， sensitivity and economy were compared， which were further used for the detection of microcystins in Melanioides. For LC-MS/MS method， the Waters XSelect HSS T3 （2.1 mm × 150 mm， 3.5 μm） was used as separation column with mobile phase of acetonitrile（0.1% formic acid） and water （0.1% formic acid）. The MS was operated in electrospray ionization（ESI） and multiple reaction monitoring mode（MRM） with linear range of 0.9965~0.9993 and relative standard deviation of 3.6%~6.1%. The limit of detection and the limit of quantitation were less than 0.54 ng/mL and 1.81 ng/mL， respectively. The recovery ranged from 73.9% to 83.4%. For DIA method， the fragment m/z 135.2 was selected as the characteristic ion with DP 60 eV and CE 55 eV. After precursor ion scanning （PreIS）， the microcystin were mainly ionized as [M+2H]2+. The comparison results of these two methods showed that the performance of LC-MS/MS was better than that of DIA， while DIA was faster in detection speed， which only cost one min to complete the determination of seven molecular species of microcystins. Finally， a total of 60 samples was analyzed by the two methods. The results showed that the positive samples were 63.3%， and the main pollution species were Mc-RR and LR. The results suggested that when the number of samples to be tested was large， DIA should be used for initial screening. For the positive samples， LC-MS/MS should be used for the secondary testing， which could effectively reduce the detection time， column loss and solvent consumption， and improve the reliability of the results. This analysis strategy can be applied to fast analysis of microcystins in water， animal， and plant samples， determine the monitoring and sampling position and frequency， the alert value， and the prevention and control， etc. This study could provide scientific basis for related departments to improve and strengthen the monitoring and management of aquatic products. It also could ensure the food safety and the development of offshore aquaculture.