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QuEChERS方法在食品中多组分农残检测中的研究进展

2016-02-05任水英

中国酿造 2016年9期
关键词:极性吸附剂乙腈

鹿 剑,任水英

(1.新疆特种设备检验研究院,新疆 乌鲁木齐 830011;2.国家农副产品监督检验中心(新疆),新疆 乌鲁木齐 830011;3.新疆大学 石油天然气精细化工教育部和自治区重点实验室,新疆 乌鲁木齐 830046)

QuEChERS方法在食品中多组分农残检测中的研究进展

鹿剑1,任水英2,3

(1.新疆特种设备检验研究院,新疆 乌鲁木齐 830011;2.国家农副产品监督检验中心(新疆),新疆 乌鲁木齐 830011;3.新疆大学 石油天然气精细化工教育部和自治区重点实验室,新疆 乌鲁木齐 830046)

QuEChERS技术自推出以来,因快速、简单、便宜、有效、可靠和安全等特点在农残分析中得以迅速发展和广泛应用。本文针对QuEChERS法在不同基质农残分析中的改进,就其在农残检测中的应用进行了综述,并对QuEChERS法在今后的应用前景以及发展方向进行了展望。

QuEChERS;样品前处理;农药残留;研究进展

农残分析中,由于样品基质复杂、待测组分含量极微,前处理方法在检测过程中起着至关重要的作用。针对复杂样品体系,常用的样品前处理技术有固相萃取法[1-2]、固相微萃取法[3]、分散固相萃取法[4]、基质分散固相萃取法(matrix solid-phase dispersion,MSPD)[5]、搅拌棒吸附萃取[6]、分散液液微萃取[7]、凝胶渗透色谱[8]、QuEChERS(Quickly,Easy,Cheap,Effective,Rugged,Safe)技术[9]等,其中QuECh-ERS技术因快速、简单、便宜、有效、可靠和安全等特点在农残分析中引起了广泛关注并得以迅速发展。本文主要针对QuEChERS法在不同基质中农残分析的改进,综述了近年来QuEChERS法在多组分农残检测方面的应用研究进展。

QuEChERS法于2002年由美国农业部东部地区研究中心的学者在第四届欧洲农药残留工作组会议上首次提出,是在固相萃取技术和MSPD技术基础上发展起来的一种针对水果和蔬菜中农药残留检测的样品前处理方法[10]。其过程可归纳为三步:(1)提取:用少量乙腈溶剂将分析物从匀浆样品中提取出来;(2)分离:加入盐析盐无水硫酸镁和氯化钠(或乙酸钠),促使液液分离;(3)净化:依据分散固相萃取原理,向乙腈层中加入净化粉,除去提取液中的共萃杂质,以减少基质效应。

QuEChERS方法适用范围广,可同时提取结构相差很大的非极性、中等极性、极性物质,包括农药[11-12]、兽药[13]、生物毒素[14]等。除了用于检测水果、蔬菜和农作物外,QuECh-ERS法还被用于蜂蜜[15]、牛奶、果汁中的农药残留检测。

1 QuEChERS的改进

QuEChERS灵活性强,已经成为世界各国残留分析技术的模板。根据目标化合物性质、样品基质、设备、分析技术的不同,研究者对QuEChERS法进行了改进,主要包括:(1)提取溶剂的改进;(2)分散固相萃取中吸附剂的选择;(3)辅助提取方式的引入。根据这些改进,QuEChERS法被发展出不同的版本,其中两个版本被定义为官方方法:(1)LEHOTAY S J等[16]采用含0.1%乙酸的乙腈为提取剂,以无水乙酸钠代替氯化钠作为盐析剂,借助乙酸-乙酸钠缓冲溶液(pH=4.8)来调节水相及有机相的酸度,提高了对酸性或碱性基质较敏感的农药的回收率,该方法被定义为AOAC法2007.01;(2)有学者[17]以乙腈为萃取剂,采用酸性较弱的柠檬酸钠-柠檬酸二钠缓冲溶液来调节提取过程中溶液的pH(5.0~5.5),经无水硫酸镁和氯化钠盐析离心分层,该方法被定义为EN 15662法。

1.1提取溶剂的选择

检测食品基质中多组分农药残留时,提取剂的选择非常关键。QuEChERS方法常用的提取溶剂包括乙腈、甲醇、乙酸乙酯、酸化甲醇、酸化乙腈。

ZHANG W等[18]以价格低廉、毒性较小的乙酸乙酯和环己烷(V/V=1∶1)为提取剂,以乙二胺N-丙基硅烷(primary secondary amine,PSA)净化粉和石墨化炭黑(graphitiacxi carhon black,GCB)为吸附剂,气相色谱-串联质谱法分析检测了黄瓜、苹果、番茄、葡萄等水果蔬菜中的啶氧菌酯、醚菌酯和肟菌酯等三种杀菌剂,并被用于土壤基质的检测中。UGARE B等[19]采用含体积分数1%甲酸的甲醇提取,建立了同时检测葡萄中的氯吡脲等4种植物生长调节剂高效液相色谱-串联质谱方法。FLORES M I等[20]以含体积分数1%乙酸的乙腈为提取剂,以超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandern mass spectrometry,UPLC-MS/MS)法同时分析检测蔬菜中的萘乙酸等6种植物生长调节剂。GOLGE O等[21]以含体积分数1%乙酸的乙腈为提取剂,采用液相色谱-质谱联用法分析检测了番茄中2,4-氯苯乙酸(2,4-D)等109种农药。LEHOTAY S J等[22]采用含1%乙酸的乙腈为提取剂,分析检测了蔬菜、水果中200多种农药,提高了酸性物质及易受基质干扰物质的回收率。LACINA O等[23]采用甲酸化乙腈为提取剂,建立了同时测定了果蔬中棒曲霉毒素等38种毒素和萘氧乙酸等288种农药的HPLC-MS/MS检测方法,提高了极性较强的酸性物质的回收率。

MOL H G J等[24]比较了三种提取剂:水-有机溶剂(乙腈、甲醇、丙酮,均含1%甲酸),从饲料及基质中同时提取农药、兽药、毒素、植物生长调节剂等172种化合物,结果表明,选择水-乙腈(1%甲酸)为提取剂时,回收率高,基质效应较低,可作为日常检测方法使用,省时省力;LEHOTAY S J等[25]比较了同时测定果蔬中多种种类农药的QuEChERS方法的三个版本,并试图用乙酸乙酯代替乙腈作为提取剂。结果表明,首创版本对受pH影响较大的物质回收率较低;采用乙酸乙酯作为提取剂时,提取的杂质较多,且吡蚜酮等多种物质回收率较低。CAMINO-SÁNCHEZ F J等[26]参照CEN版本,调整了样品与溶剂的比例,在采用气相色谱-串联质谱法同时检测果蔬中121种农药时,得到了更高的灵敏度,方法完全满足欧盟关于农药残留检测的要求。COSTA F P等[27]比较了QuEChERS法三个版本在提取桃罐头食品中10种农药时的效率,结果表明,三个版本在回收率方面无显著的区别,这可能因为对于成熟的桃子,有机酸含量降低,糖含量增加,即便未使用缓冲溶液,提取液的pH范围也在4~5之间,与使用缓冲溶液的方法(pH4.8~5.5)相差不大;该方法用基质标液和内标法解决了基质效应较大的问题。

乙腈是最常用的提取溶剂,对农药的极性要求不高,可在较宽泛的pH范围内获得较高的回收率,且溶解的非极性物质如脂肪及极性较大化合物如蛋白质、盐类、糖较少[28];同时,通过盐析作用,乙腈易与水层分离。实验中,为了延长不稳定化合物的稳定性,提高酸性物质及易受基质干扰物质的回收率,常用乙酸或甲酸将乙腈酸化。酸性萃取剂使目标化合物呈分子状态,避免了酸性化合物的水解,提高了酸性化合物及易受基质干扰物质的回收率。采用酸化乙腈作为提取溶剂拓展了QuEChERS技术的使用范围。

1.2分散固相萃取中吸附剂的选择

对于基质较复杂的样品检测,净化步骤非常重要。干扰物质的去除有利于降低检出限,增加结果准确率。净化效果主要决定于吸附剂的选择。根据待测组分以及样品中干扰基质的不同,研究者需选择不同的吸附剂。MANTZOS N等[29]以PSA为吸附剂,建立了土壤、向日葵、油菜中吡草胺、乙氧氟草醚、精喹禾灵、喹草酸、氯氰菊酯等的分析方法。WANG P等[30]以GCB为分散固相萃取吸附剂,分析检测橘子、绿茶等植物源性食品中的除草剂,当样品为杏仁和花生油时,吸附剂替换为弗洛里硅土。KOESUKWIWAT U等[31]以C18和中性铝为吸附剂,采用超高效液相色谱-电喷雾二级质谱联用技术法分析检测了大米中的13种苯氧基酸类除草剂。ZHAO H等[32]以弗洛里硅土、石墨化炭黑为吸附剂,以QuEChERS-液相色谱串联质谱法分析检测了水果蔬菜中的酞酰替苯胺酸,此方法可用于日常的检测中。KOESULWIWAT U等[33]采用MgSO4、PSA和C18为吸附剂,成功地从富含脂肪的谷物、亚麻籽、花生和面团中提取了莠去津等34种常用农药,净化效果优于凝胶渗透色谱及冷冻实验。ARIAS J L等[34]在用QuEChERS-液相色谱串联质谱法检测水稻土样中的16种农药时,比较了甲壳素,壳聚糖,硅藻土和PSA等吸附剂的提取效率和基体效应,结果表明,壳聚糖最好。BEYER A等[35]比较了不同吸附剂在检测低脂食品中多氯联苯和农药时的净化效果,结果表明,弗罗里硅土、氧化铝和NH2柱净化效果好,去除干扰物质的量最大,可保证大多数化合物的回收率高于70%;而非多孔石墨化炭黑和C18柱并没有消除基体干扰。

除了选择现有的吸附剂,自制选择性吸附剂也成为研究者的研究方向。WANG F等[36]以自制的四环素-芳烃-三嗪修饰的环芳烃超大分子为吸附剂,采用液相色谱技术,分析了水果中氯吡脲六种植物生长调节剂。ZHAO P等[37]以自制的多壁碳纳米管净化剂,分析检测了番茄及番茄制品中的乙草胺等186种残留农药。WANG Z H等[38]以自制备的多壁碳纳米管为固相萃取吸附剂,分析检测了植物样品中的萘乙酸、吲哚丁酸,结果表明,用该物质做吸附剂比C18效果好。

综上,PSA、C18、GCB在农药残留检测前处理方法中是效果较好的净化吸附剂。PSA兼具极性相互作用和较弱的阴离子交换作用,可有效从非极性样品中除去极性物质如色素、糖、有机酸等。C18产生强非极性相互作用,主要用来从极性样品中提取非极性、中等极性化合物,如脂肪酸、烯烃类、色素等大分子干扰物质。GCB主要用来除去疏水性物质如叶绿素、类胡萝卜素等[39]。实际分析中,可根据目标化合物及样品基质的不同进行选择或者配合使用。

另外,在以下两种情况下,可省去净化过程:一是采用消耗溶剂少、富集倍数及提取效率高的液相微萃取技术处理样品时,与QuEChERS技术相结合,可省去净化过程;二是样品本身干扰相对较少,且采用准确度和精密度较高的色谱-串联质谱作为分析平台时,可省去净化过程。

1.3辅助提取方式的引入

MAO X等[40]在微波辅助模式下,以乙酸乙酯为提取剂,浓缩近干后以乙腈复溶,再采用MgSO4和PSA净化粉净化,用液相色谱串联质谱技术分析了梨中的吲哚乙酸等6种植物生长调节剂,微波辅助提取技术第一次被应用在果蔬中植物生长调节剂的检测。PORORTO-FIGUEIRAP等[41]采用超声辅助QuEChERS前处理方法,采用超高效液相色谱-荧光检测器分析检测了谷物中典型的玉米赤霉烯酮,与传统的QuEChERS法相比,该方法沉析盐用量少、样品量少、提取溶剂少。ZHANG F等[42]在超声辅助条件下,以乙腈水为提取剂,以修正的QuChERS法处理样品,分析检测了豆芽中的6-苄氨基嘌呤等4种植物生长调节剂。CHO S K等[43]采用低温冷冻(-80℃)的方式使乙腈相、水相分离,以HPLC-MS/MS技术同时检测了豆芽中的多菌灵、噻菌灵、6-BA等化合物。MORENO C M等[44]将大蒜样品用液氮冷冻,研磨成粉,再用甲醇在低温(22~25℃)条件下提取,然后将提取液在-20℃的冰箱内放置3 h,分析检测了样品中的青鲜素。ESPARZA X等[45]将苹果样品冷冻贮存,以乙酸乙酯在超声浴条件下提出,浓缩复溶,检测了苹果样品中的α-萘乙酸、α-萘氧乙酸、β-萘乙酸、β-萘氧乙酸、萘乙酰胺等萘乙酸类植物生长调节剂。

辅助方法包括微波辅助提取、超声波辅助提取的引入,可提高目标化合物的提取效率;而对样品的冷冻处理减少了提取液中的基质,为后续的净化处理及分析检测提供了方便。

2 QuEChERS方法的优势

与传统方法相比,QuEChERS方法彰显出明显的优势[46-48]:(1)检测对象范围广,可同时检测极性、中等极性及非极性物质;(2)基质适用范围广,不但适用于水果、蔬菜,也被应用于蜂蜜、牛奶、果汁等样本的农药残留检测;(3)净化过程可使用不同种类吸附剂,减少基质效应;(4)净化过程中有机酸可被除去,对精密仪器影响较小;(5)回收率高,对大量极性和挥发性农药都有较高的回收率;(6)稳定性好,精密度可满足欧洲法典对食品和饲料中农药残留分析方法控制及验证程序的控制[49]。(7)省时省力,处理速度块,每30~40min可完成10~20个预先称重样品的处理;(8)提取过程消耗溶剂少,分析成本低;使用溶剂毒性小,废液少,减少环境污染;(9)样品处理过程无需特殊装置,可广泛用于小型实验室甚至可移动的实验室;(10)操作简便、步骤少,无需较多的培训和较高的技能。

3 展望

QuEChERS方法作为一种新型的广谱多残留提取净化技术,自问世以来得到迅速发展和广泛应用。与常规样品前处理技术相比,QuEChERS方法较大程度地解决了传统方法所需时间长、有毒溶剂使用量大、共存物易干扰定性和定量等问题,尤其在多残留检测方面优势明显。其提取净化介质已经渗透到各个领域,涉及水果、蔬菜、谷物、各类深加工食品以及土壤、水等。

QuEChERS灵活性强,已经成为世界各国残留分析技术的模板。由于一个分析方法可能不适用于不同的基质,实验人员可以根据分析物、基质成分不同,通过改变提取溶剂、调整不同吸附剂及其用量等手段灵活改进优化方法,达到实验目的。另外,QuEChERS和气相色谱串联质谱、液相色谱串联质谱联用法发展迅速,在环境样品及生物样品的前处理领域会有广阔的发展空间。

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Research progress of QuEChERS method in multi-pesticides residue analysis in food

LU Jian1,REN Shuiying2,3
(1.Xinjiang Uygur Autonomous Region Inspection Institute of Special Equipment,Urumqi 830011,China;2.National Quality Supervision Test Center of Agricultural Byproducts(Xinjiang),Urumqi 830011,China;3.Ministry Key Laboratory of Oil and Gas Fine Chemicals,College of Chemistry and Chemical Engineering,Xinjiang University,Urumqi 830046,China)

As a quick,easy,cheap,effective,reliable and safe sample preparation method,QuEChERS method has developed rapidly and used widely in pesticide residue analysis since its inception.The article focused on the improvement of QuEChERS method in the analysis of pesticide residues in different matrix,and summarized its application in multi-residue determination of pesticides and forecasted the bright prospect of QuEChERS method.

QuEChERS;sample preparation;pesticide residues;research progress

O656

0254-5071(2016)09-0028-05doi:10.11882/j.issn.0254-5071.2016.09.007

2016-06-08

鹿剑(1975-),男,高级工程师,本科,主要从事特种设备检验工作。

任水英(1981-),女,高级工程师,博士研究生,主要从事食品检测及相关科研工作。

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