付海濱,閆超杰,李修平,張 敏,蔣 施,徐宜宏
(1.沈陽出入境檢驗檢疫局,遼寧 沈陽 110016;2.錦州出入境檢驗檢疫局,遼寧 錦州 121013;3.濟寧出入境檢驗檢疫局,山東 濟寧 272100;4.沈陽農(nóng)業(yè)大學(xué) 工程學(xué)院,遼寧 沈陽 110866)
食品安全早已成為全世界所面臨的一個迫切需要解決的問題,食品中有害化學(xué)物質(zhì)殘留,以及病原微生物污染問題,是困擾當前食品安全的重要因素之一.食品安全若要得到保障,必須依靠完善的食品質(zhì)量監(jiān)管體系,而精準高效的檢驗方法是其中不可缺少的重要組成部分.目前,世界各國都在積極制定相關(guān)法令政策,研發(fā)更為快速、準確、靈敏的檢測方法.
在食品安全檢測過程中,樣品前處理通常是最關(guān)鍵和費時的一步.食品樣品中目標化合物的濃度很低,有大量雜質(zhì)和干擾物存在,因此只有在對目標化合物進行分離和富集后,才能用標準的分析測試方法進行檢測.食品安全檢測前處理中已報道的提取方法有[1]:索氏提取(SOX)、液-液萃取(LLE)、固相萃取(SPE)、微波輔助萃?。∕AE)、超聲輔助萃?。║E)等,但這些方法分別存在著明顯的不足:提取時間長、萃取溶劑用量多、分析人員勞動強度大、回收率及精確度不高等.1995年Richter等[2]提出了一種全新的萃取方法——加速溶劑萃取法(Accelerated Solvent Extraction,ASE),為殘留分析提供了省時、省溶劑、安全、自動化的萃取技術(shù).
目前,國內(nèi)外學(xué)者已經(jīng)開展了ASE技術(shù)在食品安全檢測中的運用等一系列研究.本文對加速溶劑萃取技術(shù)的基本原理及其在食品安全檢測技術(shù)中的應(yīng)用情況進行了綜述,從而使分析工作者更加深入了解加速溶劑萃取技術(shù)在食品安全檢測分析中的應(yīng)用及前景.
加速溶劑萃?。ˋSE)是指在較高的溫度(最高200℃)和壓力(10.3Pa)下,用有機溶劑萃取固體或半固體的自動化過程.ASE的基本原理是在高溫及加壓條件下,增加物質(zhì)溶解度和溶質(zhì)擴散率,提高萃取的效率,大大減少溶劑用量,縮短提取時間.ASE萃取過程的主要影響因素是溫度和壓力,溫度的增高能夠打斷溶劑與基質(zhì)之間的作用力(范德華力、氫鍵等),使被溶物快速從基質(zhì)中解析出來,溶劑體系溫度升高時,被提取物的溶解度隨之增大,降低了溶劑和樣品基質(zhì)之間的表面張力,使溶劑更好地進入樣品基質(zhì),有利于被萃取物與溶劑的接觸;而液體對溶質(zhì)的溶解能力遠遠大于氣體[3],升高壓力使溶劑的沸點也相應(yīng)增高,從而使溶劑在萃取的過程中始終保持液態(tài).
加速溶劑萃取(ASE)是近年廣泛應(yīng)用的樣品前處理技術(shù),與傳統(tǒng)的萃取方法相比,ASE 具有幾項顯著的優(yōu)點:①萃取時間短,僅用12~20 min即可完成;②溶劑用量少,15~45mL溶劑用量;③萃取效率高,同時使用多元溶劑萃取;④安全,全自動地進行大量樣品處理,減少了對操作者的毒害,同時ASE 萃取的整個操作處于密閉系統(tǒng),減少溶劑揮發(fā)對環(huán)境的污染,和環(huán)境的相容性好.目前,該技術(shù)已經(jīng)被美國國家環(huán)保局批準為EPA3545號標準方法.表1是幾種傳統(tǒng)的萃取方法與ASE方法的比較.
表1 傳統(tǒng)萃取方法與ASE方法的比較Table 1 Compared of traditional extraction method and ASE method
在食品安全檢測領(lǐng)域,農(nóng)、獸藥殘留是最受民生關(guān)注和檢測機構(gòu)日常開展的檢驗項目,食品中農(nóng)、獸藥種類復(fù)雜,不同種類的食品(如蔬菜、水果、肉類等)使用農(nóng)藥種類不同,一種食品還可能使用多種農(nóng)藥,因此,食品中農(nóng)、獸藥殘留檢測不僅要快速準確,而且還要實現(xiàn)多殘留同時檢測.目前,很多檢驗機構(gòu)實驗室已具備了先進的食品分析儀器,但在樣品前處理階段仍使用傳統(tǒng)的人工操作方法.傳統(tǒng)方法費時費力,往往檢測回收率比較低.近年來ASE作為新出現(xiàn)的高效、快速、安全的前處理技術(shù)得到了食品安全檢測人員的極大關(guān)注,該方法不但可以滿足同時處理大量樣品的需要,而且方法回收率較高、分析結(jié)果快速準確,同時相對標準偏差也在食品安全檢測允許的范圍內(nèi).表2為近年來主要報道的ASE 方法在農(nóng)、獸藥殘留檢測中的應(yīng)用.
表2 ASE在農(nóng)、獸藥殘留檢測中的應(yīng)用Table 2 Application of ASE in detection of pesticide and veterinary drug residue
持久性有機污染物(Persistent Organic Pollutants,簡稱POPs)指人類合成的能持久存在于環(huán)境中、通過生物食物鏈累積、并對人類健康造成有害影響的化學(xué)物質(zhì).它具備4種特性:高毒、持久、生物積累性、親脂憎水性.而位于生物鏈頂端的人類,則把這些毒性放大到了7 萬倍.近年來,以二噁英、多氯聯(lián)苯、多環(huán)芳烴為代表的持久性有機污染致癌物質(zhì)一直為世界各國政府和組織所關(guān)注.ASE方法因其快速高效在食品中持久性污染物殘留檢測中也得到了深入應(yīng)用.表3為近年來報道的ASE 方法在持久性有機污染物殘留檢測中的應(yīng)用.
表3 ASE方法在持久性有機污染物殘留檢測中的應(yīng)用及參考文獻Table 3 Application of ASE method in detection of persistent organic pollutants residue and references
加速溶劑萃?。ˋSE)技術(shù)因其具有提取效率高,操作簡單快捷的特點,目前也廣泛應(yīng)用于食品中無機污染物、防腐劑等其他種類污染物殘留檢測的前處理實驗中.實驗證明,與傳統(tǒng)的萃取方法相比,加速溶劑萃取法在回收率和提取率等方面確實有很大的優(yōu)越性,鑒于報道文獻較多,表4僅列舉幾類近年來報道的ASE 方法在其他種類污染物殘留檢測中的應(yīng)用.
表4 ASE方法在其他種類污染物殘留檢測中的應(yīng)用及參考文獻Table 4 Application of ASE method in detection of other types of pollutants residue and references
迄今為止,加速溶劑萃取技術(shù)已在農(nóng)業(yè)、環(huán)境、藥物、化工等方面得到了廣泛的應(yīng)用,在食品安全檢測領(lǐng)域加速溶劑萃取技術(shù)主要被用來萃取食品中的有毒有害物質(zhì).加速溶劑萃取技術(shù)是一種新的利用高溫高壓進行提取的技術(shù),在樣品處理中具有自動化、省時省溶劑、安全等特點,同時也可以滿足食品檢測需處理大量樣品的要求,適用于多種樣品中多種分析物的提取和富集,相信加速溶劑萃取技術(shù)在食品安全檢測領(lǐng)域具有廣闊的研究和應(yīng)用前景.
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