水产品中三类药物多残留的HPLC和UPLC-MS/MS分析方法研究
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摘要
水产品中药物残留问题是世界各国普遍关注的食品安全热点之一,建立有效的药物残留分析方法是对水产品中药物残留进行监测和控制的前提和基础。由于水产品基质的复杂性和水产养殖用药的特殊性,使水产品药物残留检测存在一些困难和问题。一方面相关法规对一些新出现或在水产养殖中新使用的药物设定了限量要求,但缺少合适的检测方法,如水产品中喹乙醇标示残留物3-甲基喹嗯啉-2-羧酸(MQCA)和阿苯达唑及其代谢物等；另一方面一些已有的多残留检测方法存在检测时间较长、前处理成本高,灵敏较低等问题,如水产品中磺胺类药物残留的检测。如何解决这些问题,满足国内外越来越严格的法规要求,是目前研究的重点和热点。解决这些问题对于提高行业检测水平,保证水产品质量安全均具有重要的意义。
本论文针对目前水产品药残检测存在的问题,以喹乙醇标示残留物MQCA、阿苯达唑及其代谢物和磺胺类药物残留等为研究对象,深入研究了水产品药物多残留的样品前处理技术和高效液相色谱(HPLC)、超液相色谱-串联质谱(UPLC-MS/MS)分析方法。在样品前处理方法研究中使用了近年来引起广泛关注的碳纳米管萃取和基质固相分散等技术,有效提高了前处理效率。在检测过程中使用了多同位素内标稀释技术,以提高方法回收率和精密度。仪器分析过程中采用UPLC进行快速色谱分离,用串联质谱进行结构解析和准确定量。
1.针对目前缺乏合适的喹乙醇标示残留物MQCA检测方法的问题建立了水产品中喹乙醇标示残留物的氢氧化钠水解-HPLC检测方法和盐酸水解-UPLC-MS/MS定量分析方法。
建立的MQCA的氢氧化钠水解-HPLC检测方法具有除杂彻底、线性范围大、仪器配备要求低等特点。方法前处理采用氢氧化钠水解,可彻底去除蛋白等杂质。方法采用普通C18柱等度洗脱进行色谱分离,紫外检测器检测。方法在4-200μg/kg添加范围内平均回收率为80.0%-86.7%；日内相对标准偏差(RSD)为3.26-6.47%,日间RSD为2.54-7.54%；方法定量限为4.0μg/kg。与普通的液液萃取和偏磷酸水解-HPLC方法相比回收率分别提高了18.3%和11.9%。
建立的MQCA盐酸水解-UPLC-MS/MS检测方法具有定量准确、分析时间短、灵敏度和精密度高等特点。针对MQCA残留在水产品基质中呈结合态,难以充分提取的问题,创新使用盐酸水解前处理方法,可有效释放并提取与基质呈结合态的MQCA。方法与碱水解和酶水解方法相比回收率分别提高了19.2%和10.4%,精密度分别提高了3.17%和1.59%。色谱分离采用UPLC梯度洗脱仅需5min,显著缩短了分析时间。利用质谱母离子和子离子扫描方法确定了合适的定性和定量特征离子,并推导了MQCA的质谱裂解过程。采用同位素标准品D4-QCA作为内标,显著降低了基质影响,提高了方法的回收率和精密度。方法的平均回收率为92.7-104.3%；日内RSD小于5.54%,日间RSD小于5.64%；方法具有较高的灵敏度,检出限(LOD)和定量限(LOQ)分别为0.1μg/kg和0.25μg/kg,显著低于目前已有的方法。利用建立的盐酸水解-UPLC-MS/MS检测方法对60个鱼肉样品进行了检测,有1个阳性样品检出。
2.利用多同位素内标稀释定量技术,在乙酸乙酯快速提取、PS-DVB固相萃取和碳纳米管萃取三种前处理方法的基础上建立了水产品中阿苯达唑及其代谢物阿苯达唑砜、阿苯达唑亚砜和阿苯达唑-2-氨基砜的三种UPLC-MS/MS多残留分析方法。
针对阿苯达唑及其三种代谢物之间的pKa值相差较大,在不同水产品中基质效应不同而导致的提取不完全、回收率相差大等问题,首次使用多同位素内标稀释定量技术,提高了方法回收率和精密度。三种同位素内标物在实验过程中与各自分析物同等稀释、浓缩和损耗,可显著缩小由分析物性质不同引起的回收率和精密度差异以及基质干扰。方法与先前报道的非那西汀内标法、艾司唑仑内标法相比回收率均有大幅提高,表现出了优异的准确度和重现性。
利用串联质谱母离子和子离子扫描方法确定了合适的定性和定量特征离子,在此基础上推导了阿苯达唑、阿苯达唑亚砜、阿苯达唑砜和阿苯达唑-2-氨基砜的质谱裂解过程。三种方法均使用UPLC进行色谱分离,可在4min内完成液-质联用分析,具有高通量分析的特点。
水产品中阿苯达唑及其代谢物的乙酸乙酯快速提取-UPLC-MS/MS定量分析方法快速、简便,适用于新鲜鱼、虾等基质相对简单的水产品。通过比较甲醇、乙腈和乙酸乙酯的提取效率,确定了在碱性条件下用乙酸乙酯提取的快速前处理方法。方法平均回收率为92.8～113.7%；日内RSD小于7.01%,日间RSD小于6.38%；LOD为0.03-0.05μg/kg, LOQ为0.1-0.2μg/kg。
利用PS-DVB固相萃取柱的亲水性基团对阿苯达唑类药物保留较强的性质,建立了水产品中阿苯达唑及其代谢物的PS-DVB固相萃取-UPLC-MS/MS定量分析方法。方法有较高的灵敏度,适合于基质复杂、脂肪含量高的鱼和鱼干等样品分析。在前处理研究中,比较了C,8. HLB、 PS-DVB固相萃取柱的效果,发现PS-DVB固相萃取柱的苯乙烯-二乙烯基苯聚合物亲水性基团对阿苯达唑类药物残留的保留最好。在此基础上对PS-DVB固相萃取的淋洗、洗脱条件进行了优化,建立了固相萃取净化方法。方法平均回收率在92.4～109.0%之间；日内RSD小于8.77%,日间RSD小于7.31%；LOD为0.02-0.04μg/kg,LOQ为0.08-0.15μg/kg。
利用多壁碳纳米管对阿苯达唑类残留特异的吸附性质,首次建立了一种基于新型材料碳纳米管萃取的阿苯达唑及其代谢物的UPLC-MS/MS检测方法。在前处理方法中研究了不同尺寸多壁碳纳米管对阿苯达唑及其代谢物的吸附和洗脱性能,开发了一种新型碳纳米管固相萃取柱,并优化了固相萃取条件。与传统的固相萃取柱相比,本研究制备的碳纳米管固相萃取柱成本仅为其十分之一,且对分析物富集和净化效果显著。由于碳纳米管高效的富集和净化效果,在建立的三种方法中碳纳米管萃取UPLC-MS/MS方法灵敏度最高。方法平均回收率在95.2～104.0%之间；日内RSD小于5.99%,日间RSD小于6.98%；LOD为0.02-0.04μg/kg, LOQ为0.06-0.12μg/kg。
利用建立的UPLC-MS/MS分析方法对100个水产样品进行了检测,有2个草鱼阳性样品和1个鳗鲡阳性样品检出。
3.为了解决目前磺胺类药物残留检测中存在的前处理过程复杂、定量不稳定和成本较高的问题,建立了水产品中磺胺类药物残留的MSPD-HPLC在线柱后衍生荧光检测方法和碳纳米管萃取-UPLC-MS/MS检测方法。
建立的水产品中磺胺类药物残留的MSPD-HPLC在线柱后衍生荧光检测方法快速、简便,具有较高的灵敏度和精密度。MSPD前处理方法采用中性氧化铝作为基质分散剂,无需分散剂的平衡和淋洗步骤,与常用的MSPD方法相比更为快速和简便。在荧光检测的基础上发展了在线柱后衍生-荧光检测方法,无需人工加入衍生试剂,缩短分析时间,并提高了方法的灵敏度和精密度。方法使用内标法定量,8种磺胺类残留平均回收率为83.8～112.4%,日内RSD小于9.79%,日间RSD小于9.28%；方法的LOD在2.0～8.0μg/kg之间,LOQ在5.0～20μg/kg之间。
建立了水产品中磺胺类药物残留的碳纳米管萃取-UPLC-MS/MS检测方法。多壁碳纳米管具有比表面积大,吸附容量大的特点,利用这一性质可对磺胺类多残留组分充分富集萃取。研究首先确定了碳纳米管的用量,然后优化了吸附洗脱条件,最终建立了一种碳纳米管萃取前处理新方法。与传统的固相萃取柱相比,碳纳米管固相萃取对磺胺多组分残留的吸附容量更大,富集和洗脱过程更为稳定。方法使用UPLC进行色谱分离,可在10min内将10种磺胺有效分离,与常规高效液相色谱法相比明显缩短了分析时间。利用串联质谱母离子和子离子扫描方法确定了合适的定性和定量特征离子。方法使用两种同位素内标进行定量,获得了较好的回收率和精密度。10种磺胺类药物在0.5～100μg/kg范围内平均回收率为82.2～117.6%；日内RSD小于11.7%,日间RSD小于12.8%；10种磺胺类药物残留的LOD在0.1～0.2μg/kg之间,LOQ在0.3～0.5μg/kg之间。
用建立的MSPD-HPLC-在线柱后衍生荧光检测法对240个水产样品进行了检测,有7个阳性样品检出。阳性样品品种包括鲈鱼、罗非鱼、大菱鲆、对虾、甲鱼等。阳性样品超标的药物为磺胺甲基异嗯唑、磺胺噻唑、磺胺甲基嘧啶和磺胺喹噁啉。
通过研究建立了水产品中三类药物残留的快速、准确、灵敏的HPLC和UPLC-MS/MS定量分析方法。各方法的准确度和精密度均符合残留分析质量控制程序的要求,定量限均满足国内外药物残留限量的要求。本研究可为水产品中药物残留的检测和监控提供分析手段和理论依据,对药物残留检测新方法开发、水产品安全评价具有重要指导意义和借鉴价值。
The issue of veterinary residues in aquatic products is one of the food safety problems throughout the world by widespread concern. Effective detection methods are the first requirement for survey and control veterinary residues. The complexity of matrices and particularity of veterinary in aquaculture, brings some difficulties for the analysis of veterinary residues. On one hand, residue limits of relevant regulations on new veterinary drugs used in aquaculture were already set, but there still lack of suitable analysis methods, for example, analysising the olaquindox marker residue methyl-3-quinoxaline-2-carboxylic acid (MQCA) and albendazole and its metabolites. On the other hand, there are still several shortages in some existing methods, such as time-consuming, higher cost and lower sensitivity, like analysis method of sulfonamides(SAs) in aquatic products. How to solve these problems, meet more and more strict regulations and requriments domestic and abroad, is the study hotspot and focus. Resolving these problems, it is great significance for heightening detecting ability and ensuring safety of aquatic products.
In this paper, sample pre-treatments, HPLC and UPLC-MS/MS methods for determination of marker substance of olaquindox, albendazole and its metabolites, SAs in aquatic product was studied. Some novel technology such as carbon nanotubes (CNTs) extraction, matrix solid-phase dispersion (MSPD) were explored to improve the extract efficient in sample pre-treatment procedure. Multi-isotope dilution technique was used to obtain better recovery and lower RSD. During the instrumental analysis, UPLC was used for rapid chromatographic separation, and tandem mass was used for structural elucidation and quantitative analysis.
1. Sodium hydroxide hydrolysis HPLC and hydrochloric acid hydrolysis UPLC-MS/MS methods were developed for the quantification of MQCA in aquatic products, aming at the lack of suitable analysis method at present.
The major advantages of sodium hydroxide hydrolysis-HPLC method include removing impurities completely, wide linear range and low requirements for analytical instruments and equipments. In this method, hydrolysis by sodium hydroxide, it was remove protein completely. Analyte was separated by LC isocratic elution mode and detected by ultraviolet detector. The average recoveries of MQCA, spiked at level of4-200μg/kg, were80.0-86.7%, with the intra-day RSD3.26-6.47%and inter-day RSD2.54-7.54%. The limit of quantitation(LOQ) for MQCA was4.0μg/kg. Compared with liquid-liquid extraction (LLE) and phosphate Acid hydrolysis-HPLC method, recoveries of the method increased by18.3%and11.9%, precision of the method increased by1.14%and0.56%, respectively.
Acid hydrolysis-UPLC-MS/MS method characterized by accurate quantification, high sensitivity, good precision and short analysis time, hydrochloric acid was used to hydrolysis and release MQCA bound protein in this method. Compared with alkaline hydrolysis and enzymatic digest method, the recoveries increased by19.2%and10.4%, precision increased by3.17%and1.59%, respectively. The chromatographic separation was achieved in less than5min by UPLC, reduced the run time significantly. MS scan and daughter scan modes was used to selected qualitative and quantitative ions, the fragmentation pathways of MQCA was also studied. Isotope internal standard D4-QCA was used to decrease the interference of matrix and increase recovery and precision. The average recoveries of MQCA were92.7-104.3%, with the intra-day and inter-day RSDs less than5.54%and5.64%, respectively. The LOD and LOQ for MQCA were0.1μg/kg and0.25μg/kg, which were lower than the existing methods. The developed method was applied to the analysis60batch of fish, one of them was confirmed positive for MQCA.
2. Three UPLC-MS/MS methods were developed to determine albendazole(ABZ), albendazole sulfoxide, albendazole sulfone and albendazole2-aminosulfone in aquatic products by using multi-isotope dilution technique.The pre-treatments of the three method were based on rapid extraction by ethyl acetate, PS-DVB SPE and CNTs extraction, respectively.
The differences of pKa values between ABZ and its metabolites induce incomplete extraction efficiency and significant difference in recoveries. The first use of internal standard quantitative technique of multi-isotope dilution to improve recovery and precision in this method. Three isotope internal standards was used to correct the matrix effect and variations in dilutions, evaporation, degradation, recovery and precision. The result shows good accuracy and reproducibility. Compared with the methods of eralier reported using estazolam and phenacetin as internal standards, the recovery of this method increased significantly.
MS scan and daughter scan modes was used to selected qualitative and quantitative ions, the fragmentation pathways of ABZ and its metabolites was also studied. The chromatographic separation was achieved in4min by UPLC, which is suitable for high-throughput analysis.
Ethyl acetate rapid extraction combind with UPLC-MS/MS method is rapid, simple and suitable for samples of fresh fish and shrimp. Three solvents, methanol, acetonitrile and ethyl acetate were tested in a side-by-side comparison. Ethyl acetate under the alkaline condition was selected as the best extraction solvent for the sample preparation. The average recoveries of the method were92.8-113.7%, with the intra-day and inter-day RSDs less than7.01%and6.38%. The LOD and LOQ for ABZ and its metabolites were in the range of0.03-0.05μg/kg and0.1-0.2μg/kg, respectively.
A PS-DVB SPE combined with UPLC-MS/MS method was developed for determination of ABZ and its metabolites in aquatic products. The method is sensitive and suitable for fish samples with complex matrix or high fat. Three types of SPE columns C18, HLB, PS-DVB were tested and compared, and PS-DVB SPE column showed the best purification effect. Then, the washing and eluting conditions were optimized. The average recoveries of the method were92.4-109.0%, with the intra-day and inter-day RSDs less than8.77%and7.31%. The LOD and LOQ for ABZ and its metabolites were in the range of0.02-0.04μg/kg and0.08-0.15μg/kg, respectively.
A novel CNTs extraction combined with UPLC-MS/MS method was developed for determination of ABZ and its metabolites based on the adsorption property of MWCNTs. The absorbing and eluting behaviour for different size of MWCNTs was studied. Furthermore, a new type of solid phase extraction column using MWCNTs as sorbent was developed, and the SPE conditions were further optimized. Compared with conventional SPE columns, the cost was only1/10, and showed better enrichment and purification effect. The method of CNTs extraction-UPLC-MS/MS shows the best sensitivity among three new methods. The average recoveries of this method were95.2-104.0%, with the intra-day and inter-day RSDs less than5.99%and6.98%. The LOD and LOQ for ABZ and its metabolites were in the range of0.02-0.04μg/kg and0.06-0.12μg/kg, respectively.
The developed ethyl acetate rapid extraction-UPLC-MS/MS method was applied to the analysis100batch of aquatic products, two grasscrab sample and one eel sample were confirmed positive.
3. MSPD-HPLC online postcolumn derivatization fluorescence detection method and CNTs SPE-UPLC-MS/MS method were developed to determine SAs in aquatic products, aiming at the issues of complex pre-treatment, inaccuracy in quantitative analysis and high cost of analysis.
MSPD-HPLC online postcolumn derivatization fluorescence detection method is rapid, simple, sensitive and with high precision, neutral alumina was used as dispersant in MSPD pre-treatment. By this method, SAs could be isolated by only one step, without the sorbent conditioning and sorbent-tissue matrix washing. Online postcolumn derivatization and fluorescence detection method was established based on HPLC-FLD method. In this method, derivatizing agent don't need to be added manually, which reduce the analysis time and improve sensitivity and precision of the method. Internal standard was used in quantitative analysis, and the average recoveries of this method were83.8-112.4%, with the intra-day and inter-day RSDs less than9.79%and9.28%. The LOD and LOQ for MQCA were in the range of2.0-8.0μg/kg and5.0-20μg/kg, respectively.
A CNTs SPE-UPLC-MS/MS method was developed for determination of ten SAs by using the MWCNTs'property of high surface area and adsorption. First, the amount of CNTs was ascertained, then the absorbing and eluting conditions were optimized. Finally, the pre-treament method of CNTs SPE was established. Compared with conventional SPE columns, CNTs SPE showed bigger adsorption capacity, more stable properties of enrichment and elution. The chromatographic separation was achieved in10min by UPLC, reduced the run time significantly. The average recoveries of ten SAs, spiked at level of0.5-100μg/kg, were82.2-117.6%, with the intra-day and inter-day RSDs less than11.7%and12.8%. The LOD and LOQ for SAs were in the range of0.1-0.2μg/kg and0.3-0.5μg/kg, respectively.
The developed MSPD-HPLC method by online postcolumn derivatization and fluorescence detection was applied to the analysis240batch of aquatic products, seven samples were confirmed positive. The species of positive samples were perch, tilapia, turbot, shrimp and turtle. The positive drugs were sulfamethoxazole, sulfathiazole, sulfamerazine and sulfaquinoxaline.
HPLC and UPLC-MS/MS methods for determination of three kinds of veterinary residues in aquatic products were developed in this paper. The accuracy and precision of these methods all keep in accordance with Method Validation and Quality Control Procedures, and all the LOQs meet the demands of MRL prescribed by domestic and abroad regulations. These methods are suitable for the determination and confirmation of veterinary residues in aquatic products and can be used for residue control programs. It also has a great value for development of new analytical methods and evaluation on safety of aquatic products.
本论文针对目前水产品药残检测存在的问题,以喹乙醇标示残留物MQCA、阿苯达唑及其代谢物和磺胺类药物残留等为研究对象,深入研究了水产品药物多残留的样品前处理技术和高效液相色谱(HPLC)、超液相色谱-串联质谱(UPLC-MS/MS)分析方法。在样品前处理方法研究中使用了近年来引起广泛关注的碳纳米管萃取和基质固相分散等技术,有效提高了前处理效率。在检测过程中使用了多同位素内标稀释技术,以提高方法回收率和精密度。仪器分析过程中采用UPLC进行快速色谱分离,用串联质谱进行结构解析和准确定量。
1.针对目前缺乏合适的喹乙醇标示残留物MQCA检测方法的问题建立了水产品中喹乙醇标示残留物的氢氧化钠水解-HPLC检测方法和盐酸水解-UPLC-MS/MS定量分析方法。
建立的MQCA的氢氧化钠水解-HPLC检测方法具有除杂彻底、线性范围大、仪器配备要求低等特点。方法前处理采用氢氧化钠水解,可彻底去除蛋白等杂质。方法采用普通C18柱等度洗脱进行色谱分离,紫外检测器检测。方法在4-200μg/kg添加范围内平均回收率为80.0%-86.7%；日内相对标准偏差(RSD)为3.26-6.47%,日间RSD为2.54-7.54%；方法定量限为4.0μg/kg。与普通的液液萃取和偏磷酸水解-HPLC方法相比回收率分别提高了18.3%和11.9%。
建立的MQCA盐酸水解-UPLC-MS/MS检测方法具有定量准确、分析时间短、灵敏度和精密度高等特点。针对MQCA残留在水产品基质中呈结合态,难以充分提取的问题,创新使用盐酸水解前处理方法,可有效释放并提取与基质呈结合态的MQCA。方法与碱水解和酶水解方法相比回收率分别提高了19.2%和10.4%,精密度分别提高了3.17%和1.59%。色谱分离采用UPLC梯度洗脱仅需5min,显著缩短了分析时间。利用质谱母离子和子离子扫描方法确定了合适的定性和定量特征离子,并推导了MQCA的质谱裂解过程。采用同位素标准品D4-QCA作为内标,显著降低了基质影响,提高了方法的回收率和精密度。方法的平均回收率为92.7-104.3%；日内RSD小于5.54%,日间RSD小于5.64%；方法具有较高的灵敏度,检出限(LOD)和定量限(LOQ)分别为0.1μg/kg和0.25μg/kg,显著低于目前已有的方法。利用建立的盐酸水解-UPLC-MS/MS检测方法对60个鱼肉样品进行了检测,有1个阳性样品检出。
2.利用多同位素内标稀释定量技术,在乙酸乙酯快速提取、PS-DVB固相萃取和碳纳米管萃取三种前处理方法的基础上建立了水产品中阿苯达唑及其代谢物阿苯达唑砜、阿苯达唑亚砜和阿苯达唑-2-氨基砜的三种UPLC-MS/MS多残留分析方法。
针对阿苯达唑及其三种代谢物之间的pKa值相差较大,在不同水产品中基质效应不同而导致的提取不完全、回收率相差大等问题,首次使用多同位素内标稀释定量技术,提高了方法回收率和精密度。三种同位素内标物在实验过程中与各自分析物同等稀释、浓缩和损耗,可显著缩小由分析物性质不同引起的回收率和精密度差异以及基质干扰。方法与先前报道的非那西汀内标法、艾司唑仑内标法相比回收率均有大幅提高,表现出了优异的准确度和重现性。
利用串联质谱母离子和子离子扫描方法确定了合适的定性和定量特征离子,在此基础上推导了阿苯达唑、阿苯达唑亚砜、阿苯达唑砜和阿苯达唑-2-氨基砜的质谱裂解过程。三种方法均使用UPLC进行色谱分离,可在4min内完成液-质联用分析,具有高通量分析的特点。
水产品中阿苯达唑及其代谢物的乙酸乙酯快速提取-UPLC-MS/MS定量分析方法快速、简便,适用于新鲜鱼、虾等基质相对简单的水产品。通过比较甲醇、乙腈和乙酸乙酯的提取效率,确定了在碱性条件下用乙酸乙酯提取的快速前处理方法。方法平均回收率为92.8～113.7%；日内RSD小于7.01%,日间RSD小于6.38%；LOD为0.03-0.05μg/kg, LOQ为0.1-0.2μg/kg。
利用PS-DVB固相萃取柱的亲水性基团对阿苯达唑类药物保留较强的性质,建立了水产品中阿苯达唑及其代谢物的PS-DVB固相萃取-UPLC-MS/MS定量分析方法。方法有较高的灵敏度,适合于基质复杂、脂肪含量高的鱼和鱼干等样品分析。在前处理研究中,比较了C,8. HLB、 PS-DVB固相萃取柱的效果,发现PS-DVB固相萃取柱的苯乙烯-二乙烯基苯聚合物亲水性基团对阿苯达唑类药物残留的保留最好。在此基础上对PS-DVB固相萃取的淋洗、洗脱条件进行了优化,建立了固相萃取净化方法。方法平均回收率在92.4～109.0%之间；日内RSD小于8.77%,日间RSD小于7.31%；LOD为0.02-0.04μg/kg,LOQ为0.08-0.15μg/kg。
利用多壁碳纳米管对阿苯达唑类残留特异的吸附性质,首次建立了一种基于新型材料碳纳米管萃取的阿苯达唑及其代谢物的UPLC-MS/MS检测方法。在前处理方法中研究了不同尺寸多壁碳纳米管对阿苯达唑及其代谢物的吸附和洗脱性能,开发了一种新型碳纳米管固相萃取柱,并优化了固相萃取条件。与传统的固相萃取柱相比,本研究制备的碳纳米管固相萃取柱成本仅为其十分之一,且对分析物富集和净化效果显著。由于碳纳米管高效的富集和净化效果,在建立的三种方法中碳纳米管萃取UPLC-MS/MS方法灵敏度最高。方法平均回收率在95.2～104.0%之间；日内RSD小于5.99%,日间RSD小于6.98%；LOD为0.02-0.04μg/kg, LOQ为0.06-0.12μg/kg。
利用建立的UPLC-MS/MS分析方法对100个水产样品进行了检测,有2个草鱼阳性样品和1个鳗鲡阳性样品检出。
3.为了解决目前磺胺类药物残留检测中存在的前处理过程复杂、定量不稳定和成本较高的问题,建立了水产品中磺胺类药物残留的MSPD-HPLC在线柱后衍生荧光检测方法和碳纳米管萃取-UPLC-MS/MS检测方法。
建立的水产品中磺胺类药物残留的MSPD-HPLC在线柱后衍生荧光检测方法快速、简便,具有较高的灵敏度和精密度。MSPD前处理方法采用中性氧化铝作为基质分散剂,无需分散剂的平衡和淋洗步骤,与常用的MSPD方法相比更为快速和简便。在荧光检测的基础上发展了在线柱后衍生-荧光检测方法,无需人工加入衍生试剂,缩短分析时间,并提高了方法的灵敏度和精密度。方法使用内标法定量,8种磺胺类残留平均回收率为83.8～112.4%,日内RSD小于9.79%,日间RSD小于9.28%；方法的LOD在2.0～8.0μg/kg之间,LOQ在5.0～20μg/kg之间。
建立了水产品中磺胺类药物残留的碳纳米管萃取-UPLC-MS/MS检测方法。多壁碳纳米管具有比表面积大,吸附容量大的特点,利用这一性质可对磺胺类多残留组分充分富集萃取。研究首先确定了碳纳米管的用量,然后优化了吸附洗脱条件,最终建立了一种碳纳米管萃取前处理新方法。与传统的固相萃取柱相比,碳纳米管固相萃取对磺胺多组分残留的吸附容量更大,富集和洗脱过程更为稳定。方法使用UPLC进行色谱分离,可在10min内将10种磺胺有效分离,与常规高效液相色谱法相比明显缩短了分析时间。利用串联质谱母离子和子离子扫描方法确定了合适的定性和定量特征离子。方法使用两种同位素内标进行定量,获得了较好的回收率和精密度。10种磺胺类药物在0.5～100μg/kg范围内平均回收率为82.2～117.6%；日内RSD小于11.7%,日间RSD小于12.8%；10种磺胺类药物残留的LOD在0.1～0.2μg/kg之间,LOQ在0.3～0.5μg/kg之间。
用建立的MSPD-HPLC-在线柱后衍生荧光检测法对240个水产样品进行了检测,有7个阳性样品检出。阳性样品品种包括鲈鱼、罗非鱼、大菱鲆、对虾、甲鱼等。阳性样品超标的药物为磺胺甲基异嗯唑、磺胺噻唑、磺胺甲基嘧啶和磺胺喹噁啉。
通过研究建立了水产品中三类药物残留的快速、准确、灵敏的HPLC和UPLC-MS/MS定量分析方法。各方法的准确度和精密度均符合残留分析质量控制程序的要求,定量限均满足国内外药物残留限量的要求。本研究可为水产品中药物残留的检测和监控提供分析手段和理论依据,对药物残留检测新方法开发、水产品安全评价具有重要指导意义和借鉴价值。
The issue of veterinary residues in aquatic products is one of the food safety problems throughout the world by widespread concern. Effective detection methods are the first requirement for survey and control veterinary residues. The complexity of matrices and particularity of veterinary in aquaculture, brings some difficulties for the analysis of veterinary residues. On one hand, residue limits of relevant regulations on new veterinary drugs used in aquaculture were already set, but there still lack of suitable analysis methods, for example, analysising the olaquindox marker residue methyl-3-quinoxaline-2-carboxylic acid (MQCA) and albendazole and its metabolites. On the other hand, there are still several shortages in some existing methods, such as time-consuming, higher cost and lower sensitivity, like analysis method of sulfonamides(SAs) in aquatic products. How to solve these problems, meet more and more strict regulations and requriments domestic and abroad, is the study hotspot and focus. Resolving these problems, it is great significance for heightening detecting ability and ensuring safety of aquatic products.
In this paper, sample pre-treatments, HPLC and UPLC-MS/MS methods for determination of marker substance of olaquindox, albendazole and its metabolites, SAs in aquatic product was studied. Some novel technology such as carbon nanotubes (CNTs) extraction, matrix solid-phase dispersion (MSPD) were explored to improve the extract efficient in sample pre-treatment procedure. Multi-isotope dilution technique was used to obtain better recovery and lower RSD. During the instrumental analysis, UPLC was used for rapid chromatographic separation, and tandem mass was used for structural elucidation and quantitative analysis.
1. Sodium hydroxide hydrolysis HPLC and hydrochloric acid hydrolysis UPLC-MS/MS methods were developed for the quantification of MQCA in aquatic products, aming at the lack of suitable analysis method at present.
The major advantages of sodium hydroxide hydrolysis-HPLC method include removing impurities completely, wide linear range and low requirements for analytical instruments and equipments. In this method, hydrolysis by sodium hydroxide, it was remove protein completely. Analyte was separated by LC isocratic elution mode and detected by ultraviolet detector. The average recoveries of MQCA, spiked at level of4-200μg/kg, were80.0-86.7%, with the intra-day RSD3.26-6.47%and inter-day RSD2.54-7.54%. The limit of quantitation(LOQ) for MQCA was4.0μg/kg. Compared with liquid-liquid extraction (LLE) and phosphate Acid hydrolysis-HPLC method, recoveries of the method increased by18.3%and11.9%, precision of the method increased by1.14%and0.56%, respectively.
Acid hydrolysis-UPLC-MS/MS method characterized by accurate quantification, high sensitivity, good precision and short analysis time, hydrochloric acid was used to hydrolysis and release MQCA bound protein in this method. Compared with alkaline hydrolysis and enzymatic digest method, the recoveries increased by19.2%and10.4%, precision increased by3.17%and1.59%, respectively. The chromatographic separation was achieved in less than5min by UPLC, reduced the run time significantly. MS scan and daughter scan modes was used to selected qualitative and quantitative ions, the fragmentation pathways of MQCA was also studied. Isotope internal standard D4-QCA was used to decrease the interference of matrix and increase recovery and precision. The average recoveries of MQCA were92.7-104.3%, with the intra-day and inter-day RSDs less than5.54%and5.64%, respectively. The LOD and LOQ for MQCA were0.1μg/kg and0.25μg/kg, which were lower than the existing methods. The developed method was applied to the analysis60batch of fish, one of them was confirmed positive for MQCA.
2. Three UPLC-MS/MS methods were developed to determine albendazole(ABZ), albendazole sulfoxide, albendazole sulfone and albendazole2-aminosulfone in aquatic products by using multi-isotope dilution technique.The pre-treatments of the three method were based on rapid extraction by ethyl acetate, PS-DVB SPE and CNTs extraction, respectively.
The differences of pKa values between ABZ and its metabolites induce incomplete extraction efficiency and significant difference in recoveries. The first use of internal standard quantitative technique of multi-isotope dilution to improve recovery and precision in this method. Three isotope internal standards was used to correct the matrix effect and variations in dilutions, evaporation, degradation, recovery and precision. The result shows good accuracy and reproducibility. Compared with the methods of eralier reported using estazolam and phenacetin as internal standards, the recovery of this method increased significantly.
MS scan and daughter scan modes was used to selected qualitative and quantitative ions, the fragmentation pathways of ABZ and its metabolites was also studied. The chromatographic separation was achieved in4min by UPLC, which is suitable for high-throughput analysis.
Ethyl acetate rapid extraction combind with UPLC-MS/MS method is rapid, simple and suitable for samples of fresh fish and shrimp. Three solvents, methanol, acetonitrile and ethyl acetate were tested in a side-by-side comparison. Ethyl acetate under the alkaline condition was selected as the best extraction solvent for the sample preparation. The average recoveries of the method were92.8-113.7%, with the intra-day and inter-day RSDs less than7.01%and6.38%. The LOD and LOQ for ABZ and its metabolites were in the range of0.03-0.05μg/kg and0.1-0.2μg/kg, respectively.
A PS-DVB SPE combined with UPLC-MS/MS method was developed for determination of ABZ and its metabolites in aquatic products. The method is sensitive and suitable for fish samples with complex matrix or high fat. Three types of SPE columns C18, HLB, PS-DVB were tested and compared, and PS-DVB SPE column showed the best purification effect. Then, the washing and eluting conditions were optimized. The average recoveries of the method were92.4-109.0%, with the intra-day and inter-day RSDs less than8.77%and7.31%. The LOD and LOQ for ABZ and its metabolites were in the range of0.02-0.04μg/kg and0.08-0.15μg/kg, respectively.
A novel CNTs extraction combined with UPLC-MS/MS method was developed for determination of ABZ and its metabolites based on the adsorption property of MWCNTs. The absorbing and eluting behaviour for different size of MWCNTs was studied. Furthermore, a new type of solid phase extraction column using MWCNTs as sorbent was developed, and the SPE conditions were further optimized. Compared with conventional SPE columns, the cost was only1/10, and showed better enrichment and purification effect. The method of CNTs extraction-UPLC-MS/MS shows the best sensitivity among three new methods. The average recoveries of this method were95.2-104.0%, with the intra-day and inter-day RSDs less than5.99%and6.98%. The LOD and LOQ for ABZ and its metabolites were in the range of0.02-0.04μg/kg and0.06-0.12μg/kg, respectively.
The developed ethyl acetate rapid extraction-UPLC-MS/MS method was applied to the analysis100batch of aquatic products, two grasscrab sample and one eel sample were confirmed positive.
3. MSPD-HPLC online postcolumn derivatization fluorescence detection method and CNTs SPE-UPLC-MS/MS method were developed to determine SAs in aquatic products, aiming at the issues of complex pre-treatment, inaccuracy in quantitative analysis and high cost of analysis.
MSPD-HPLC online postcolumn derivatization fluorescence detection method is rapid, simple, sensitive and with high precision, neutral alumina was used as dispersant in MSPD pre-treatment. By this method, SAs could be isolated by only one step, without the sorbent conditioning and sorbent-tissue matrix washing. Online postcolumn derivatization and fluorescence detection method was established based on HPLC-FLD method. In this method, derivatizing agent don't need to be added manually, which reduce the analysis time and improve sensitivity and precision of the method. Internal standard was used in quantitative analysis, and the average recoveries of this method were83.8-112.4%, with the intra-day and inter-day RSDs less than9.79%and9.28%. The LOD and LOQ for MQCA were in the range of2.0-8.0μg/kg and5.0-20μg/kg, respectively.
A CNTs SPE-UPLC-MS/MS method was developed for determination of ten SAs by using the MWCNTs'property of high surface area and adsorption. First, the amount of CNTs was ascertained, then the absorbing and eluting conditions were optimized. Finally, the pre-treament method of CNTs SPE was established. Compared with conventional SPE columns, CNTs SPE showed bigger adsorption capacity, more stable properties of enrichment and elution. The chromatographic separation was achieved in10min by UPLC, reduced the run time significantly. The average recoveries of ten SAs, spiked at level of0.5-100μg/kg, were82.2-117.6%, with the intra-day and inter-day RSDs less than11.7%and12.8%. The LOD and LOQ for SAs were in the range of0.1-0.2μg/kg and0.3-0.5μg/kg, respectively.
The developed MSPD-HPLC method by online postcolumn derivatization and fluorescence detection was applied to the analysis240batch of aquatic products, seven samples were confirmed positive. The species of positive samples were perch, tilapia, turbot, shrimp and turtle. The positive drugs were sulfamethoxazole, sulfathiazole, sulfamerazine and sulfaquinoxaline.
HPLC and UPLC-MS/MS methods for determination of three kinds of veterinary residues in aquatic products were developed in this paper. The accuracy and precision of these methods all keep in accordance with Method Validation and Quality Control Procedures, and all the LOQs meet the demands of MRL prescribed by domestic and abroad regulations. These methods are suitable for the determination and confirmation of veterinary residues in aquatic products and can be used for residue control programs. It also has a great value for development of new analytical methods and evaluation on safety of aquatic products.
引文
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