TWI696817B - 用於化合物分析之樣品前處理的淨化裝置及應用淨化裝置的快篩式樣品前處理方法 - Google Patents
用於化合物分析之樣品前處理的淨化裝置及應用淨化裝置的快篩式樣品前處理方法 Download PDFInfo
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Abstract
一種用於化合物分析之樣品前處理的淨化裝置及應用淨化裝置的快篩式樣品前處理方法,快篩式樣品前處理方法主要是先粉碎待檢測物,然後取粉碎後的待檢測物混合溶劑與鹽類試劑形成溶液,接者過濾與分離溶液的液體與固體物質,再利用淨化裝置同步輸出且淨化取樣後的液體;淨化裝置包含移液組件與過濾管,過濾管內部具有淨化劑,透過移液組件吸取微量體積的液體,然後再讓被吸取的液體經由過濾管的淨化劑輸出並同步完成淨化,達成精準定量取樣且快速淨化的功效。
Description
本發明與檢測方法有關,特別是指一種用於化合物分析之樣品前處理的淨化裝置及快篩式樣品前處理方法。
為了監控農產品的農藥殘留問題,各種不同方式的農藥分析方法被應用於農業生產及市售食品之檢測工作,例如早期使用比色法檢測農藥DDT,或是薄層層析法可檢測多重殘留,乃至於利用氣相層析技術等等都曾是重要的管控方式。
目前農產品或食品的農藥殘留檢測大致可分為生化法及化學法兩大基本類型,生化法以酵素反應或抗體結合為基理,可利用較為簡易之設備及處理步驟,對特定類群之農葯品項進行快速之篩檢。化學法多以層析質譜之儀器分析法為主,透過高速均質、溶劑萃取、分配、取樣、淨化、吹乾及回溶等步驟(及相關處理設備)獲得樣品淨化萃取液,再以氣/液相層析質譜儀分析。化學法雖然建置成本昂貴,步驟複雜且耗時較長,但因可檢出更多農藥殘留、更低定量極限、可精準定性及定量分析,目前各國都仍以質譜化學法之檢測結果為執法及管理的依據。
要讓農藥分析方法更為快速且可適用於多種不同農作物,目前常見的是先應用QuEChERS樣品前處理方法,再搭配液相層析串聯質譜 (LC-MS/MS)及氣相層析串聯質譜(GC-MS/MS)等作為農藥殘留檢測之主要分析工具。我國食品藥物管理署於2012 年提出的檢測多重農藥殘留方法,亦是採用前述QuEChERS方法且使用美國FDA 使用之醋酸緩衝溶液進行萃取,後搭配GC-MS/MS及LC-MS/MS分析。
雖然前述QuEChERS前處理方法已較為便利,但其仍須執行許多萃取、分層、取樣及淨化等步驟,在分析時效與應用需要較長的檢測時間,難以完全配合各類農產品的上市時效。
因此,本發明的主要目的乃在於提供一種快篩式樣品前處理方法,其可更為快速且簡便地檢測化合物。
本發明的另一目的則在於提供一種用於化合物分析之樣品前處理的淨化裝置,其可快速且精準定量的完成取樣與淨化等前處理步驟。
為達成前述目的,本發明提供用於化合物樣品前處理方法的淨化裝置,包含一移液組件與一過濾管;該移液組件具有一末端,該移液組件吸取微量體積的取樣液,並可將該取樣液移出該末端;該過濾管具有一第一端口與一第二端口,該過濾管內部設一液體通道連通該第一端口與該第二端口,該液體通道內部設有淨化劑,該過濾管以該第一端口可分離地設於該移液組件的末端,藉此自該末端被移出的該液體經由該液體通道通過該淨化劑輸出並淨化至該第二端口,達成可快速且精準定量的完成取樣與淨化等前處理步驟之功效。
本發明提供的快篩式樣品前處理方法,包含有以下步驟:1. 均質:粉碎待檢測物;2. 萃取:取粉碎後的該待檢測物混合溶劑與鹽類試劑形成溶液;3. 過濾:分離該溶液的液體與固體物質;4. 淨化:利用上述淨化裝置取得淨化後的該液體。
有關於本發明所提供的詳細特點將於後續的實施方式詳細說明中予以描述。然而,本領域技術人員應能瞭解,詳細說明以及實施本發明所列舉的特定實施例僅是用於說明,並非用以限制本發明的權利要求保護範圍。
首先要說明的是,本發明可廣泛應用於檢測各種化合物,例如用於農作物的殘留農藥或動物用的殘留藥物等,本領域技術人員能瞭解本實施方式與權利請求範圍的說明用語包含特定技術方式的上位概念,不限於描述內容,不限制應用領域,也並非限制於特定的檢測技術特徵。
如第1圖所示,本發明所提供用於檢測化合物的快篩式樣品前處理方法,主要包含下列步驟:
1. 均質:如第2圖所示,粉碎待檢測的農產作物,本發明主要是透過家用型調理機10粉碎農產作物之後取得體積均勻且細小的樣品14,家用型調理機10除了方便取得與使用,而且可應用於不同種類與植物形式的農產作物以外,更重要的是用以增加樣品的接觸表面積。
2. 萃取:如第3圖及第4圖所示,用50ml萃取離心管12盛裝10克粉碎後的樣品14,接著混合加入乙腈溶劑10ml,再倒入鹽類試劑,直接以手上下搖晃離心管12約30秒,讓樣品14與溶劑之間產生液液分配萃取效果。
3. 過濾:如第5圖所示,先將濾紙22設置呈長容器狀,然後將濾紙22直接置入上述萃取離心管12內部,樣品溶液的液體即可透過濾紙22過濾流入濾紙22中央的內部空間,樣品溶液的固體物質則隔絕於濾紙22外部。
4. 淨化:如第6圖所示,利用一淨化裝置30淨化前述樣品溶液過濾後的液體,淨化裝置30包含一移液組件32與一過濾管34,於本較佳實施例的移液組件32係以正位移式移液組件(Positive displacement pipette)為例,當然也可選用其他具有準確吸取微量液體的移液組件。移液組件32具有一末端33,如第7圖所示,先只利用移液組件32的末端33從前述樣品溶液過濾後的液體吸取出預定且微量體積的取樣液,然後在移液組件32的末端33直接套接過濾管34,再利用移液組件32將取樣液推移出末端33並且經由過濾管34流出即可取得淨化後的取樣液。
如第8圖所示,於本較佳實施例的過濾管34具有一第一端口37與一第二端口38,過濾管34內部設一液體通道40連通第一端口37與第二端口38,液體通道40內部鄰近第二端口38位置設有一過濾件39,本較佳實施例的過濾件39以棉花為例。過濾件39由一設於液體通道40內部的環狀定位件36限位於過濾管34內部,於本較佳實施例的定位件36是體積較小的管體,過濾管34的液體通道40內部於過濾件39上方填設淨化劑42,如第10圖所示,過濾管34以第一端口37可分離地套設於移液組件32的末端33,如第11圖所示,自末端33被移出之取樣液經由液體通道40通過淨化劑42輸出並淨化至第二端口38,即可盛裝於測試瓶50,再由後續的質譜測定方法檢驗出溶液內的化合物成分。
再者,如第9圖所示,本發明所提供的過濾管也可改由兩上下串接的管體60所組成,第一端口61形成在位於上方的管體60頂端,第二端口63形成在位於下方的管體60底端,兩管體60之間連通形成出液體通道40,過濾件62位於液體通道40內部且介於第一端口61與第二端口63之間,淨化劑42填設於液體通道40內部且介於第一端口61與過濾件62之間。
藉由上述淨化裝置與樣品前處理方法,本發明具有以下多項增進的技術功效:
1. 由於淨化裝置的過濾管可分離地搭配正位移式移液組件一起使用,正位移式移液組件單一次的液體移出過程即可同步完成取樣與淨化步驟,不需要習用的振盪及離心程序,也就不需要相對應的設備及處理時間,如第12圖所示,經驗證過本發明相較於台灣公告方法(五)可簡化整體前處理的時間約47%,亦即約由32分鐘減為17分鐘。
2. 過濾管內部的淨化劑依照檢測樣品的特性而變化調整,不需要再改變過濾管的形式種類,有利於制定標準且統一的快篩檢測規範。
3. 本發明利用例如家用型調理機的輕量化粉碎機即可處理樣品,不需要習用的高功率粉碎機,可方便在一般實驗室、各個不同的產、銷或展售現場實地執行即時的分析檢測前處理,並獲得與習用方法相似之測定值。
4. 過濾過程只需要利用濾紙,減少且簡化了振盪及離心步驟也能得到與習用方法相似乾淨之萃取溶液。
5. 綜合前述的技術特徵,本發明所取得的前處理樣品可配合後續的液相層析質譜儀建構出快速篩檢的檢測方法,如第13圖所示,本發明同樣可用於測試164項農藥藥劑,而如第14圖及第15圖所示,本發明分別用於檢測萵苣與芥藍菜,以台灣公告方法(五)與本案的快篩式樣品前處理方法配合液相層析質譜儀分析之結果比較,本案所測得之藥劑品項與台灣公告方法(五)一致,殘留量亦可相比較,幾乎無假陰性結果。
10‧‧‧家用型調理機
12‧‧‧離心管
14‧‧‧樣品
22‧‧‧濾紙
30‧‧‧淨化裝置
32‧‧‧移液組件
33‧‧‧末端
34‧‧‧過濾管
36‧‧‧環狀定位件
37‧‧‧第一端口
38‧‧‧第二端口
39‧‧‧過濾件
40‧‧‧液體通道
42‧‧‧淨化劑
60‧‧‧管體
61‧‧‧第一端口
62‧‧‧過濾件
63‧‧‧第二端口
第1圖為本發明一較佳實施例的流程圖。 第2圖至第7圖為本發明一較佳實施例的製法示意圖。 第8圖為本發明一較佳實施例之過濾管的剖視圖。 第9圖類同於第8圖,主要顯示過濾管的另一實施態樣。 第10圖為本發明一較佳實施例之淨化裝置的示意圖。 第11圖為本發明一較佳實施例之淨化裝置的使用示意圖。 第12圖為本發明一較佳實施例的時間比較圖。 第13圖為本發明一較佳實施例的總離子層析圖。 第14圖及第15圖為本發明一較佳實施例的檢驗結果圖。
Claims (5)
- 一種用於化合物樣品前處理方法的淨化裝置,包含:一移液組件,具有一末端,該移液組件直接吸取過濾後的取樣液,並再將該取樣液移出該末端;以及一過濾管,具有一第一端口與一第二端口,該過濾管內部設一液體通道連通該第一端口與該第二端口,該液體通道內部設有淨化劑與一位於該淨化劑與該第二端口之間的過濾件,該過濾管以該第一端口可分離地設於該移液組件的末端,藉以讓自該末端移出的該取樣液經由該液體通道通過該淨化劑與該過濾件輸出並淨化至該第二端口;其中,該過濾管包括兩上下串接的管體,該第一端口形成於其中一管體頂端,該第二端口形成於另一該管體底端,該兩管體之間連通形成出該液體通道,該過濾件位於該液體通道內部且介於該第一端口與該第二端口之間,該淨化劑位於該液體通道內部且介於該第一端口與該過濾件之間。
- 如請求項1所述用於化合物樣品前處理方法的淨化裝置,其中該過濾件由一設於該液體通道內部的定位件限位於該過濾管內部。
- 如請求項1所述用於化合物樣品前處理方法的淨化裝置,其中該移液組件為正位移式移液組件。
- 一種過濾管,主要用於化合物樣品前處理方法的淨化裝置,該過濾管具有一第一端口與一第二端口,該過濾管內部設一液體通道連通該第一端口與該第二端口,該過濾管包括兩上下串接的管體,該第一端口形成於其中一該管體頂端,該第二端口形成於另一該管體底端,該兩管體之間連通形成出該液體通道,該液體通道內部設有淨化劑與一位於該淨化劑與該第二端口之間的 過濾件,該淨化劑位於該液體通道內部且介於該第一端口與該過濾件之間,該過濾管以該第一端口可分離地設於一具有取樣液的移液組件,藉以讓自該移液組件移出的該取樣液經由該液體通道通過該淨化劑與該過濾件輸出並淨化至該第二端口。
- 一種快篩式樣品前處理方法,包含:a:均質:粉碎待檢測物;b.萃取:取粉碎後的該待檢測物混合溶劑與鹽類試劑形成溶液;c.過濾:利用一濾紙分離該溶液的液體與固體物質;以及d.淨化:利用上述請求項1至請求項3任一淨化裝置的移液組件直接吸取過濾後的該取樣液,並且再由該淨化裝置的同一該移液組件推動該取樣液通過該過濾管淨化該取樣液。
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