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  • Title: [Sulfonated magnetic graphite carbon nitride solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry for screening malachite green and leucomalachite green in freshwater fish].
    Author: Meng EQ, Nian QX, Li F, Zhang QP, Xu Q, Wang CM.
    Journal: Se Pu; 2023 Aug; 41(8):673-682. PubMed ID: 37534554.
    Abstract:
    Malachite green (MG) and its metabolite, leucomalachite green (LMG), exert toxic effects on the human body. The use of these dyes is illegal, but they are still detected in aquatic products. Freshwater fish are aquatic products with the high non-qualified rates. Therefore, the sensitive screening of MG and LMG in freshwater fish is of great importance to ensure the safety of aquatic products. Owing to the low contents of MG and LMG in fish and the complex matrix of actual samples, sample preparation is required before detection to purify impurities and enrich the target compounds. Graphite carbon nitride (GCN), a polymer material composed of C, N, and H, has good chemical and thermal stability, a large specific surface area, and a large number of active sites. It has a wide range of application prospects in adsorption and can be used in food safety testing when compounded with Fe3O4 to form magnetic graphite carbon nitride (MGCN). In this study, sulfonated magnetic graphite carbon nitride (S-MGCN) was prepared by further functionalizing MGCN with sulfonic acid. After characterization by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR), and vibrating sample magnetometry (VSM), a magnetic solid-phase extraction (MSPE) method based on S-MGCN was established to extract MG and LMG from freshwater fish. The targets were screened using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Following sulfonic acid functionalization, S-MGCN showed increased electrostatic interactions based on the MGCN adsorption mechanism, which includes hydrogen bonds and π-π interactions; thus, its adsorption efficiency was significantly improved. The matrix effects were -42.21% and -33.77% before functionalization, -11.40% and -7.84% after functionalization, thus confirming that S-MGCN has significant matrix removal ability. Given that S-MGCN demonstrated excellent efficiency as an MSPE adsorbent, the adsorption conditions for S-MGCN were optimized. The optimal conditions were as follows: adsorbent dosage, 15 mg; adsorption time, 2 min; solution pH, 5; and ionic strength, not adjusted. Under these conditions, the adsorption efficiency of S-MGCN could reach 94.2%. Different organic solvents were used to elute adsorbed MG and LMG, and the desorption efficiency peaked when 1%(v/v) ammonia acetonitrile was used as the elution solvent. The elution volume was also optimized, and a maximum desorption efficiency of 93.2% was obtained when 1 mL of 1%(v/v) ammonia acetonitrile was added to S-MGCN. The limits of detection (LODs) and quantification (LOQs) of the two targets were determined at signal-to-noise ratios (S/N) of 3 and 10, respectively. The LODs and LOQs were 0.075 μg/kg and 0.25 μg/kg, respectively. The linear ranges of the two target compounds were 0.25-20.0 μg/kg with correlation coefficients (r) greater than 0.998. To assess accuracy and precision, we prepared spiked samples at three levels (low, medium, and high) with six parallel samples per level (n=6). The recoveries ranged from 88.8% to 105.9%. The intra- and inter-day relative standard deviations were 5.4%-13.7% (n=6) and 3.3%-11.1% (n=3), respectively. Compared with the national standard method, the proposed method features simpler sample pretreatment procedures, less use of organic reagents (5 mL), and a shorter extraction time (2 min); moreover, the method does not require complicated elution steps, and the eluent can be directly analyzed by UPLC-MS/MS. The test results of actual samples were consistent with those obtained via the national standard method, thus confirming the practical feasibility of the developed method. The proposed MSPE method based on S-MGCN is an efficient and environmentally friendly method that could provide a new methodological reference for the sensitive screening of MG and LMG in actual samples. 孔雀石绿(MG)及其代谢产物隐色孔雀石绿(LMG)在水产品中禁止检出,但违规使用行为屡禁不止,淡水鱼为抽检不合格率最高的水产品,因此,淡水鱼中MG和LMG的灵敏筛检对水产品食用安全非常重要。该工作研制了磺酸化磁性氮化碳(S-MGCN)材料,在考察其作为优良的磁性固相萃取(MSPE)吸附剂的基础上,以空白样品的加标回收率为指标,对S-MGCN用量、吸附时间、溶液pH、离子强度、洗脱溶液种类和体积等影响因素进行了优化,建立了基于S-MGCN的MSPE方法以提取淡水鱼中的MG及LMG,结合超高效液相色谱-串联质谱(UPLC-MS/MS),进行目标物的灵敏筛检。研究表明,S-MGCN对MG和LMG具有良好的吸附效率(94.2%以上),且净化样品基质效果好。该方法样品前处理简便,有机试剂的使用量少(5 mL),萃取时间短(2 min)。对两种目标物的检出限和定量限分别为0.075 μg/kg和0.25 μg/kg,灵敏度高于国标法(0.5 μg/kg);在0.25~20.0 μg/kg内线性关系良好(r>0.998),方法的回收率为88.8%~105.9%,日内和日间的相对标准偏差(RSD)均小于14%,准确度和精密度与国标法相当。最后,通过实际样品的检测验证了该方法的实际应用可行性。该文建立的基于S-MGCN的MSPE方法是一种高效环保的方法,为实际样品孔雀石绿和隐色孔雀石绿的灵敏筛检提供了新的方法学参考。
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