TW201121893A - Detection kit of melamine and detection method thereof - Google Patents

Detection kit of melamine and detection method thereof Download PDF

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Publication number
TW201121893A
TW201121893A TW98146433A TW98146433A TW201121893A TW 201121893 A TW201121893 A TW 201121893A TW 98146433 A TW98146433 A TW 98146433A TW 98146433 A TW98146433 A TW 98146433A TW 201121893 A TW201121893 A TW 201121893A
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Taiwan
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melamine
sample
mixture
test reagent
transition metal
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TW98146433A
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Chinese (zh)
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TWI412494B (en
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Chun-Nan Kuo
Shou-Nan Li
Shao-I Yan
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Ind Tech Res Inst
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  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

A detection kit of melamine comprises an organic solvent and a transition metal complex which is dissolved in the organic solvent. When the detection kit of melamine is applied to detect a melamine of a sample, a detection method comprising: first, mixing the detection kit of melamine with the sample and standing for forming a supernatant and a precipitate. Next, collecting the supernatant, and observing a color of the supernatant by visual method and analyzing the supernatant by a UV-VIS spectrophotometer. Finally, comparing an analysis result and confirming the sample is contaminated with the melamine or not.

Description

201121893 六、發明說明: 【發明所屬之技術領域】 方法,特別是一種可 本發明係有關於一種檢驗試劑及其檢驗 快速檢測三聚氰胺之檢驗試劑及其檢驗方法 【先前技術】 三聚氰胺(mdamine)是-種有機化工的中間產物,盆主要用令 是和帽產找合反應,形錢具有硬度高、耐纽耐輕等= 性的三聚氰胺帽樹脂(又稱美耐皿樹脂或聚尿樹脂),而被廣泛的 應用於木材、塑膠、塗料、皮革、電料產業中。 然而’由於三聚氰胺同時具有白色單斜晶體的外形以及幾乎 無味、形似蛋白粉的特性,散相對於蛋白質而言具有更高比例 的氮f子(三聚氰胺的含氮量為66%,而蛋白質的平均含氮量則僅 有I】6%)。因此在近年來,被不法商人使用於食品添加劑的用途上, 以製k出食品中蛋白f含量較高的假像。其原因在於在食品工 /、通吊疋藉由飢氏定氮法㈤ddahi meth〇d)或杜馬斯法(D_s test)^^仃蛋自f含量的檢測。這兩種方法並非直接對食品令的蛋 質含量進行檢測,而是以食品中的總氮含量來反推蛋白質 量。 氮曰因此,當食品中含有三聚氰胺時,將能大幅提升食品中的總 物=進而造成高蛋白質含量的假像。最終導致如2007年美國寵 Ύ染事件和2〇〇8年中國毒奶粉事件等嚴重的食品安全事故 的發生〇,卷人挪, 田八锻在長期攝取三聚氰胺後,可能造成生殖能力損害、 201121893 膀胱或腎結石、膀胱癌等疾病。 • 自他上述食品安全事故爆發後,目前在食品安全的檢驗上, 會進一步的對食品中三聚氰胺的含量進行檢驗,以確保食用上的 安全性。目前在食品工業中用於檢驗三聚氰胺的方法,大致上分 為:高效能液態層析-紫外光法(HPLCUV)、氣相層析質譜儀法 (GC/MS)以及液相層析串連質譜儀法(LC/MS/MS)等檢驗方法。這 些檢驗方法的共通點在於,所有待測定樣品在分析前均需經過前 籲處理程序,如萃取、震盈、離心、過滤及層析等一連串嚴謹費時 的萃取與純化程序後,接著再以紫外光光譜儀或質譜儀進行定性/ 疋里为析。其中,前處理程序通常需花費丨至2小時的操作時間, 而之後儀器分析的時間則大約僅需1〇分鐘左右就能得到分析社 果。 、、° 因此’無論是高效能液態層析-紫外光法、氣相層析質譜儀法 以絲相層析_連質譜儀法,經過相#娜賴作程序才能 #獲得制定樣品的分析結果,因此存在有分析時間過長以及分析 成本過高躲點。並且,在這些檢财法巾,若祕理程序沒做 好,則容易造成制定樣品中的师太多,秘f後序的處理速 度以及降低分析結果的精確度。此外,在這些方法中所使用的儀 器設備,由於其價格昂貴而僅存在於某些特定的研究單位(或實驗 室)。因此’對於食品令三聚氰胺含量的檢驗分析,只能透過這些 特定的研究單位進行分析,進而增加這些研究單位的工作㈣ 量。此不僅會f彡響分騎果的料度,並场崎錄驗效率。 201121893 方嫩有前在食品工業中,應用於三聚氰胺的檢驗 有==Γ。因此,對於食品工業而言,如何能快速且 =題:驗食品中是否含有三聚氰胺,仍是目前業界締解決的 【發明内容】 上關題’本發明提供—種三聚氰胺檢賴劑及其檢 2如改良f知對於三聚氰胺的檢驗方法,需經過如萃取、 震盛、離心縣及層_嚴謹㈣的萃取與純化程序後,才能 以分析勤雜進彳爾,㈣分析輪長及分析效率不 麵問題。朗時改良f知檢驗方法中,所使用之分析儀器的取 传困難’導録驗作業必需於特定的研究單位進行,所造成分析 率大幅降低的問題。 本發明揭露-種三聚氰胺檢驗試劑,其包含有—有機溶劑以 及-過渡金屬錯合物。過渡金屬錯合物聽解於核溶劑中,且 過渡金屬錯合物具有-帶正電的金射⑽子。過渡金屬錯合物 係藉由此帶正電的金射心原子與三聚氰胺的胺基相結合,而形 成一過渡金屬化合物。 本發明另揭露-種三聚氰胺之檢驗方法,包含有下列步驟: 提供-三聚氰胺檢驗試劑及—樣品。其中,三聚氰胺檢驗試劑包 3 -有機溶劑及-溶解於此有機溶獅過渡金屬錯合物。接著, 將二聚氰驗驗試瓶樣^進行混合使形成混絲。崎靜置 201121893 μ液’使形成上清液及沉_ 可見光光譜_行峡,^ 场液如紫外光_ 雄圖進行比tf # 綺圖。接著提供一標準光 。曰圖進盯輯,㈣崎樣品巾衫含有三聚 品光谱圖中具有-三聚氰胺吸收蜂。 疋、, a氛胺_劑,係由有機溶劑及過渡金 屬2物所_。#應_三聚氰_檢驗時,可藉由過渡金屬 錯,物所帶有的帶正電金屬中心原子與三聚氰胺的胺基結合,之201121893 VI. Description of the invention: [Technical field to which the invention pertains] The method, in particular, the invention relates to a test reagent and a test reagent thereof for rapidly detecting melamine and a test method thereof [Prior Art] Melamine (mdamine) is - An intermediate product of organic chemicals, the main purpose of the pot is to find a reaction with the hat, and the melamine cap resin (also known as melamine resin or polyurethane) with high hardness and resistance to lightness and resistance It is widely used in wood, plastic, paint, leather and electrical materials industries. However, because melamine has both the appearance of a white monoclinic crystal and the almost odorless, protein-like character, it has a higher proportion of nitrogen f (relative to protein with nitrogen) (melamine has a nitrogen content of 66%, while protein average The nitrogen content is only I]6%). Therefore, in recent years, it has been used by unscrupulous traders for the use of food additives to produce artifacts with high levels of protein f in foods. The reason for this is that the food product/, the sling is tested by the hunger method (five) ddahi meth〇d) or the Dumas method (D_s test). Instead of directly detecting the egg content of the food, these two methods reverse the amount of protein by the total nitrogen content of the food. Nitrogen, therefore, when food contains melamine, it will greatly increase the total amount of food in the food = and thus cause high protein content. Eventually, such as the occurrence of serious food safety accidents such as the US pet taint incident in 2007 and the Chinese tainted milk powder incident in 2008, the volatility of the people, Tian Ba Forging may cause reproductive damage after long-term intake of melamine, 201121893 Bladder or kidney stones, bladder cancer and other diseases. • Since the outbreak of the food safety incident mentioned above, the melamine content of the food has been further tested on food safety inspection to ensure the safety of food. The current methods for testing melamine in the food industry are broadly classified into high performance liquid chromatography-ultraviolet light (HPLCUV), gas chromatography mass spectrometry (GC/MS), and liquid chromatography tandem mass spectrometry. Test method such as instrument method (LC/MS/MS). The commonality of these test methods is that all samples to be tested need to undergo a pre-call process, such as extraction, shock, centrifugation, filtration and chromatography, after a series of rigorous and time-consuming extraction and purification procedures, followed by UV. The optical spectrometer or mass spectrometer is used for qualitative/influence analysis. Among them, the pre-processing program usually takes up to 2 hours of operation time, and then the instrument analysis time takes about 1 minute to get the analysis result. Therefore, 'whether it is high-performance liquid chromatography-ultraviolet light method, gas chromatography mass spectrometry method by silk chromatography-to-mass spectrometry method, through the phase #娜赖作程序# can obtain the analysis results of the sample Therefore, there is a long time for analysis and the cost of analysis is too high. Moreover, in these money-checking methods, if the secret procedure is not done well, it is easy to cause too many teachers in the sample preparation, the processing speed of the order, and the accuracy of the analysis result. Moreover, the instrumentation equipment used in these methods is only present in certain specific research units (or laboratories) due to its high price. Therefore, the analysis of the melamine content of food can only be analyzed through these specific research units, thereby increasing the work of these research units (IV). This will not only affect the quality of the ride, but also record the efficiency. 201121893 Before the tenderness of the food industry, the application to melamine was ==Γ. Therefore, for the food industry, how can it be quick and = question: whether the test contains melamine, is still the industry to solve the problem of the invention. [Top] 'The present invention provides a kind of melamine detector and its inspection 2 For example, if the method for testing melamine is to be subjected to the extraction and purification procedures such as extraction, shaking, centrifugation, and layer _ rigorous (four), it is necessary to analyze the dilute and enter the sputum, and (4) analyze the wheel length and the analysis efficiency. . In the Langshi improvement method, the analysis instrument used is difficult to transfer. The guidance recording operation must be carried out in a specific research unit, resulting in a significant reduction in the analysis rate. The present invention discloses a melamine test reagent comprising an organic solvent and a transition metal complex. The transition metal complex is listened to in a nuclear solvent, and the transition metal complex has a positively charged gold (10) sub. The transition metal complex is formed by combining a positively charged gold core atom with an amine group of melamine to form a transition metal compound. The invention further discloses a method for testing melamine, comprising the steps of: providing a melamine test reagent and a sample. Among them, the melamine test reagent package 3 - organic solvent and - dissolved in the organic lion transition metal complex. Next, the chlorination test bottle samples are mixed to form a mixed yarn. Stagnation set 201121893 μ liquid 'to make the supernatant and sink _ visible spectrum _ line gorge, ^ field liquid such as ultraviolet light _ male figure to compare tf # 绮 map. A standard light is then provided. In order to enter the line, the (4) Saki sample towel has a trimeric spectrogram with a melamine-absorbing bee.疋,, a amine amine _ agent, is composed of organic solvents and transition metals. #应_Cyanide_Inspection, by a transition metal error, the positively charged metal center atom carried by the substance is combined with the amine group of melamine.

後再經由二餘胺檢驗試劑_色變換,或經由料光·可見光光 譜儀的檢測,而得到樣品中含有三聚氰胺的檢驗結果。由於在檢 驗的過程中,待測定樣品不需經過繁雜的前處理程序,並且不需 使用昂貴的檢驗儀器’如高效液相層儀及f譜儀等,因此除了可 有效的簡化檢驗流程及增加檢驗效率外,朗時能大幅節省檢驗 分析的操作成本。 以上之關於本發明内容之說明及以下之實施方式之說明係用 •以示範與解釋本發明之原理,並且提供本發明之專利申請範圍更 進一步之解釋。 【實施方式】 本發明之一實施例所揭露之三聚氰胺檢驗試劑,包括一有機 溶劑及一過渡金屬錯合物。其中,有機溶劑係選自丙酮、乙醇、 異丙醇等極性有機溶劑’過渡金屬錯合物可為但不限定於石 肖酸銅 (Copper(II) nitrate hydrate,Cu(N03)2’xH20)及硝酸鈷(c〇balt(II) nitrate hydrate,Co(N〇3)2 · xH2〇)等,並具有一帶正電之金屬中心原 201121893 子。過渡金屬錯合物係溶解於有機溶劑中,足過渡金屬錯合物於 三聚氰胺檢驗試射的含量為2.G〜3.G重量百分比(wt%)。 請參閱「第1圖」所示,當本發明之所揭露之三聚 氰胺檢驗試劑應用於樣品中三聚氰胺之檢驗時,首先提供本實施 例之三聚氰胺檢驗試劑(S11G)。同時,提供—樣品(si2Q),樣品可 為膨鬆劑或奶鱗顧於食品工業的添加物或產物。接著將:聚 氰胺檢驗試劑與樣品進行混合,使形成混合液(si3G),其中樣品於 混合液中的含量為18〜19 wt.%。‘錢,以上下方式或以震 盪器(voretx)在每分鐘30〜50轉(rpm)的轉速下,搖晃、混合3〜5分 鐘’使二聚氰胺檢驗試劑與樣品均勻混合。於混合完畢後,將混 合液於室溫下靜置1〜5分鐘’使樣品巾與有機溶财相容的物質 沉澱’而使齡祕成-上清液(supematant)及—峨物⑻· 接著,吸取上清液並填充於一石英比色管(cuvette)中,然後將 此石英比色管置入於紫外光_可見光光譜儀 spectrophotometer)中進行測定,以獲得一樣品光譜圖(sl5〇)。最 後,提供一標準光譜圖,並比對標準光譜圖與樣品光譜圖,藉以 判斷樣品中是否含有三聚氰胺^若樣品巾含有三聚氰胺,則在樣 品光譜圖中會具有一三聚氰胺吸收峰(816〇)。其原因在於,當含有 二聚氰胺的樣品與三聚氰胺檢驗試劑混合而形成混合液時,三聚 氰胺所具有的胺基(-NH2)會與過渡金屬錯合物所具有之帶正電的 金屬中心原子結合,進而形成一過渡金屬化合物。因此,利用紫 外光-可見光光譜儀進行檢驗時,會在樣品光譜圖上出現胺基的吸 201121893 收峰,而表示樣品中含有三聚氰胺。 * 此外,如「第2圖」所示,在本發明之其他實施例中,當三 聚氰胺檢驗試劑中所使用的過渡金屬錯合物為硝酸銅時,在靜置 混合液的步驟(S140)後,可進一步觀察混合液的顏色變化,並依據 混合液所呈現的顏色判斷混可品中是否含有三聚氰胺(si4〗)。當樣 品中未摻雜有三聚氰胺時,混合液係呈現紫色。 因此,在本發明所揭露之三聚氰胺之檢驗方法中,除了可透 # 過备、外光-可見光光譜儀檢驗樣品中是否含有三聚氰胺外,更可依 據二聚氰胺檢驗試劑與樣品混合後所形成之混合液的顏色,於第 -時間判斷樣品枝遭受三聚氰胺的污染。此碰可以節省樣品 的檢驗時間,並可同時簡化後續的檢驗操作步驟,而大幅提高檢 驗效率和降低檢驗成本。 請參閱「第3圖」,在本發明之另—實_所揭露的三聚氮胺 之檢驗H巾’在樣^與三聚驗檢驗__進行混合⑻冲前先 •提供一有機溶劑’此有機溶劑與三聚氰胺檢驗試劑中所使用的有 機溶劑相同或具有相容性,並且㈣品以叫6机%的含量添加 於有機溶劑中。同時,以上下搖動的方式或以震細薦⑻在每 分鐘3〇〜5〇轉(啊)的轉速下,混合3〜5分鐘,使樣品與有機溶劑 均勻混合,而形成-待測物(S121)。接著,將三聚氰胺檢驗試劑以 Π 19 wt’/。的3里加人於酬物巾,並同樣以上下搖動的方式或 以震堡器—tx)在每分鐘30〜5〇轉㈣的轉速下混合3〜5分 鐘,使三聚氰胺檢驗試劑與待測物均句混合而形成一混合液。於 201121893 混合完畢後,將混合液於室溫下靜置K5分鐘,使樣品令與有機 溶劑不相容的帅跳,秘絲齡彡成—上絲(哪函㈣及 一沉;殿物(SI40)。 之後及取上/月液並填充於一石英比色管(c·此)中,然後將 此石英比色管置入於紫外光_可見光光譜儀 spectrophotome㈣中進行測定,以獲得一樣品光譜圖(si5〇)。同 時’將此樣品光譜圖與-標準光譜圖進行比對,以判斷樣品中是 否含有三聚氰胺(S160)。 因此’本發賴揭露之三聚氰胺之檢驗方法,在檢驗前不需 對樣品進行如萃取及純化等前處理程序,只需將樣品與本發明所 揭露之二聚氰胺檢驗試劑混合後,即能以紫外光可見光光譜儀進 行檢驗,或者是透過混合後的顏色變換來判斷樣品中是否含有三 聚氰胺。因此,有效簡化樣品的檢驗流程以及大幅縮短樣品的檢 驗時間。同時,由於不需使用高效能液態層析儀、氣相層析質譜 儀或液相層析串連質譜儀等昂貴儀器,因此使本發明所揭露之檢 驗方法可普遍、廣泛的應用於一般檢驗環境中,並大幅提升檢驗 效率及降低檢驗成本。 以下結合如下列實施例對本發明進行更為詳細的說明,但本 發明的保5蔓範圍並不限於下述實施例。 實施例1 : 首先’製備三聚氰胺檢驗試劑:將硝酸銅(Copper(II) nitrate hydrate’ Cu(N03)2.xH20)錯合物加入裝有丙酮(acetone)之燒杯後攪 201121893 拌約3〜5分鐘,至硝酸銅錯合物完全溶解後備用。其中,硝酸銅 錯合物之含量約為2.0〜3.0 wt.%。 接著’製備含有不同三聚氰胺濃度的樣品: A樣品(不含三聚氰胺):取不含三聚氰胺之膨鬆劑^ 加入含有两嗣的玻璃樣品甑後,蓋上蓋子並以上下搖動方式使之 充份混合,搖動時間約為3〜5分鐘,其中不含三聚氰胺之膨鬆劑 的含量約為14〜16 wt.% ; • B樣品(含10鹏三聚氰胺):將三聚氰胺加入不含三聚氰胺 之膨鬆劑中,配製出含10 ppm三聚氰胺膨鬆劑。之後,再將含ι〇 ppm二聚氰胺膨鬆劑加人含有_的玻璃樣品瓶後,蓋上蓋子並 以上下搖動方式使之充份混合,搖動時間約為3〜5分鐘其中含 10ppm二聚氰胺膨鬆劑的含量約為14〜10 wt.% ;以及 C樣品(含2 ppm三聚氰胺):取樣品B中所配製而成的含1〇 ppm三聚氰轉鬆劑’以重量比例制加人不含三聚氰胺膨鬆 參劑’並使一者充份混合後得到含2 ppm三聚氰胺膨鬆劑。之後, 將此含2 ppm:聚氰麟鬆劑加人含有的玻璃樣品瓶後蓋 上蓋子並以上下搖動方式使之充份混合,搖動時間約為3分鐘, 其中含2 0口111二聚氰胺膨鬆劑的含量約為14〜16界(%。 • 於三聚氰胺檢驗試劑與含有不同三聚氰胺濃度的樣品配製完 成後’以2 ml玻璃滴管抽取三聚氰胺檢驗試劑,並添加於a樣品、 樣σ及(^樣时中使二聚氰胺檢驗試劑在各個樣品中具有17〜19 wt%的含量。接著,分別將樣品瓶蓋上蓋子,並以上下搖動方式 11 201121893 使三聚氰胺檢驗試劑分別與A樣品、B樣品和c樣 , 搖動時間約為3分鐘。鈇彳羞, 刀此口 r主r㈣ 以静置約5分鐘以得到上層為澄清的 =二樣品及α樣品。接著,分別抽取A1樣品、m樣品及 樣4上清液’並分職人石英比色管巾。之後,以紫外光_ 可見光光譜儀(可_波_為·〜_咖(奈米胸裝有不同 上T液的石英比色管進行檢驗。分別測量ai樣品、則樣品及α 樣时的波長吸收度’並使用㈣做為測量時的空白值樣品 (祕)。實驗結果如「第4Α圖」至「第4c圖」所示,「第4Α圖」 為Α1樣品(不含三聚氰胺,Cu+NH4C〇3)之樣品光譜圖,由於其不 ^有三聚氰胺,故在此做為一標準光譜圖;「第4B圖」為m樣品 (含10 ppm三聚氰胺,Cu+NH4C〇3+melamine)的樣品光譜圖;以 及第4C圖」為C1樣品(含2 PPm三聚氰胺,Cu+NH4C03+melamine) 的樣品光譜圖。 比較「第4A圖」、「第4B圖」和「第4C圖」,其結果顯示, 在B1樣品及C1樣品的樣品光譜圖中,分別在波長約為_瞧 以上的可見光範圍具有一三聚氰胺吸收峰(如「第4B圖」和「第 4C圖」所不),且其強度相較於不含三聚氰胺的A1樣品(在此波長 的吸收度趨近於0)為高。因此,藉由比較「第4A圖」、「第4B圖」 和「第4C圖」即可快速判斷所測定的樣品中是否含有三聚氰胺。 此外’除了以紫外光-可見光光譜儀進行檢測外,另可以目視 檢測的方式’藉由觀察三聚氰胺檢驗試劑與樣品混合後的双層混 12 201121893 合液之顏色變換,可判斷樣品中是否含有三聚氰胺。 在三聚氮胺檢驗試劑與樣品混合後,Ai樣品' m樣品和C1 «之間的顏色變換尚不明顯(未圖示)。如「第5圖」所示 找=双層混合液在靜置約35分鐘後,未含有三餘_ ^樣 品觀為紫外’而不同於則樣品和α樣品。因此,可藉由目視 檢測的方法立即得知樣品中是否含有三聚氰胺。 實施例2 : • *先’製備三聚氰胺檢驗試劑:將確酸銅錯合物加入裝有丙 酮之燒杯後麟約3〜5分鐘,至雜銅錯合物完全溶解後備用。 其中’硝酸銅錯合物之含量約為2 〇〜3 〇 wt%。 接著,製備含有不同三聚氰胺濃度的樣品: D樣品(不含三聚氰胺):取不含三聚氰胺之奶粉加入含有丙购 的玻璃樣品織’蓋上蓋子並以上下搖動方式使之充份混合,搖 動時間約為3〜5分鐘,其中不含三聚氰胺之奶粉的含量約為14〜16 ^ wt.% ; E樣品(含1〇 ppm三聚氰胺):將三聚氰胺加入不含三聚氰胺 之奶粉中,配製出含l〇ppm三聚氰胺奶粉。之後,再將含川即^^ 二聚氰胺奶粉加入含有丙酮的玻璃樣品瓶後,蓋上蓋子並以上下 搖動方式使之充份混合,搖動時間約為3〜5分鐘,其中含1〇ppm 二聚氰胺奶粉的含量約為14〜16 wt.% ;以及 F樣品(含2 ppm三聚氰胺,Cu+NH4C03+melamine):取樣品 E中所配製而成的含lOppm三聚氰胺奶粉,以重量比例原則加入 13 201121893 不含三聚氰胺奶粉,並使二者充份混合後_含a _三聚氮胺 奶粉。之後,將此含2 ppm三聚氰胺奶粉加人含有_的玻璃樣 品瓶後,蓋上蓋子並以上下搖動方式使之充份混合,搖動時間約 為3分鐘’其t含2PPm三聚氣胺奶粉的含量約為14〜16机%。 於三聚氰胺檢驗試劑與含有不同三聚氣胺濃度的樣品配製完 成後’以2 ml玻璃滴管抽取三聚氰胺檢驗試劑,並添加於d樣品、 E樣品及F樣品中’使三聚氰胺檢驗試劑在各個樣品中具有 wt%的含量。同時,分別於D樣品、E樣品及F樣品中添加膨鬆 劑’使膨鬆劑在各個樣品中的含量介於8.5〜9 5机%,藉以模擬市 售之奶類產品。接著,分別將樣品瓶蓋上蓋子,並以上下搖動方 式使二聚氰私檢驗試劑分別與D樣品、e樣品和F樣品充份混人, 搖動時間約為3分鐘。紐’靜置約5分伽得到上層為澄清的 上清液以及下層為奶粉及膨鬆劑沉澱物的双層混合液而分別形 成D1樣品(不含三聚氰胺’ Cu+NH4C〇3)、E1樣品(含1〇卯瓜三聚 氰胺’ ai+NH4C03+melamine)及F1樣品(含1〇 ppm三聚氰胺,Thereafter, the test results of melamine in the sample were obtained by means of a dihydroamine test reagent_color conversion or by a light-visible spectrophotometer. Since the sample to be tested does not need to go through complicated pretreatment procedures during the inspection process, and does not need to use expensive inspection instruments such as high performance liquid layer analyzer and f spectrometer, it can effectively simplify the inspection process and increase In addition to the test efficiency, Langshi can significantly reduce the operating costs of inspection and analysis. The above description of the present invention and the following description of the embodiments of the present invention are intended to illustrate and explain the principles of the invention. [Embodiment] A melamine test reagent disclosed in one embodiment of the present invention comprises an organic solvent and a transition metal complex. Wherein, the organic solvent is selected from polar organic solvents such as acetone, ethanol, and isopropanol. The transition metal complex may be, but not limited to, copper (II) nitrate hydrate, Cu (N03) 2' x H20. And cobalt nitrate (c〇balt(II) nitrate hydrate, Co(N〇3)2 · xH2〇), etc., and has a positively charged metal center original 201121893. The transition metal complex is dissolved in an organic solvent, and the content of the transition metal complex in the melamine test is 2. G~3. G weight percent (wt%). Referring to the "Fig. 1", when the melamine test reagent disclosed in the present invention is applied to the test of melamine in the sample, the melamine test reagent (S11G) of the present embodiment is first provided. At the same time, a sample (si2Q) is provided, which may be a leavening agent or a milk scale additive or product of the food industry. Next, the melamine test reagent is mixed with the sample to form a mixed solution (si3G) in which the content of the sample in the mixed solution is 18 to 19 wt.%. ‘Money, the above method or shaking at a speed of 30 to 50 revolutions per minute (rpm), shake and mix for 3 to 5 minutes' to uniformly mix the melamine test reagent with the sample. After the mixing is completed, the mixture is allowed to stand at room temperature for 1 to 5 minutes to "precipitate the sample towel and the organic solvent-compatible substance" to make the age-supplement (supematant) and - sputum (8)· Next, the supernatant is aspirated and filled in a quartz cuvette, and then the quartz colorimetric tube is placed in a spectrophotometer to obtain a sample spectrum (sl5〇). . Finally, a standard spectrum is provided and the standard and sample spectra are compared to determine if the sample contains melamine. If the sample contains melamine, it will have a melamine absorption peak (816 〇) in the sample spectrum. The reason is that when a sample containing melamine is mixed with a melamine test reagent to form a mixed solution, the amine group (-NH2) of the melamine and the positively charged metal center atom of the transition metal complex compound The combination further forms a transition metal compound. Therefore, when using the UV-Vis spectrometer for inspection, the amine-based absorption of the 201121893 peak appears on the sample spectrum, indicating that the sample contains melamine. * In addition, as shown in "Fig. 2", in another embodiment of the present invention, when the transition metal complex used in the melamine test reagent is copper nitrate, after the step of standing the liquid mixture (S140) The color change of the mixed solution can be further observed, and whether the melamine (si4) is contained in the mixed product is judged according to the color of the mixed liquid. When the sample is not doped with melamine, the mixture appears purple. Therefore, in the method for testing melamine disclosed in the present invention, in addition to the permeable and external light-visible spectrometer for testing whether the sample contains melamine, it may be formed by mixing the melamine test reagent with the sample. The color of the mixture was judged at the first time to be contaminated with melamine. This collision saves the inspection time of the sample and simplifies the subsequent inspection steps, which greatly improves the inspection efficiency and reduces the inspection cost. Please refer to "Fig. 3", in the inspection of the triazamine disclosed in the present invention, the H-belt' is mixed with the trimer test __ (8) before the rushing to provide an organic solvent. This organic solvent is the same as or compatible with the organic solvent used in the melamine test reagent, and (4) is added to the organic solvent at a content of 6% by volume. At the same time, the above method of shaking or mixing (8) at a speed of 3 〇 5 rpm (ah) per minute, mixing for 3 to 5 minutes, the sample is uniformly mixed with the organic solvent to form a test object ( S121). Next, the melamine test reagent was Π 19 wt'/. 3 Riga people pay for the towel, and also shake the way or shake the ball - tx) at a speed of 30~5 rpm (four) per minute for 3 to 5 minutes to make the melamine test reagent and the test object The homogenous sentences are mixed to form a mixed solution. After the mixing is completed in 201121893, the mixture is allowed to stand at room temperature for 5 minutes, so that the sample is incompatible with the organic solvent, and the silky age is smashed into a silk (which is a letter (four) and a sink; SI40). Afterwards and taking the upper/month liquid and filling it in a quartz colorimetric tube (c· this), the quartz colorimetric tube is placed in the ultraviolet light-visible spectrophotometer (4) to obtain a sample spectrum. Figure (si5〇). At the same time, 'this sample spectrum is compared with the standard spectrum to determine whether the sample contains melamine (S160). Therefore, the test method for the melamine disclosed in this issue does not need to be tested before the test. The sample is subjected to a pretreatment process such as extraction and purification, and the sample can be tested by ultraviolet light visible spectrometer after mixing with the melamine test reagent disclosed in the present invention, or by color conversion after mixing. Determine whether the sample contains melamine, thus effectively simplifying the sample inspection process and greatly reducing the inspection time of the sample. At the same time, because high-performance liquid chromatography, gas chromatography is not required Expensive instruments such as mass spectrometers or liquid chromatography tandem mass spectrometers, so that the inspection method disclosed by the present invention can be widely and widely applied in a general inspection environment, and the inspection efficiency is greatly improved and the inspection cost is lowered. EXAMPLES The present invention will be described in more detail, but the scope of the present invention is not limited to the following examples. Example 1: First, 'preparation of melamine test reagent: copper (II) nitrate hydrate' Cu (N03) 2.xH20) The complex compound is added to a beaker containing acetone (acetone) and then stirred for 21 to 3 minutes for about 3 to 5 minutes until the copper nitrate complex is completely dissolved, and the content of the copper nitrate complex is about It is 2.0~3.0 wt.%. Then 'prepare the sample with different melamine concentration: A sample (without melamine): take the melamine-free leavening agent ^ Add the glass sample containing two crucibles, cover and top Shake well to make it fully mixed, shaking time is about 3~5 minutes, the content of melamine-free leavening agent is about 14~16 wt.%; • B sample (including 10 Peng melamine) Add melamine to the melamine-free leavening agent to prepare a 10 ppm melamine leavening agent. Then, add ι〇ppm melamine leavening agent to the glass vial containing _, and then cover. And the mixture is mixed in the above shaking manner, and the shaking time is about 3 to 5 minutes, wherein the content of the 10 ppm melamine leavening agent is about 14 to 10 wt.%; and the C sample (containing 2 ppm of melamine): Take 1 〇ppm of melamine translucent agent prepared in sample B, add melamine bulking agent in a weight ratio, and mix one by one to obtain 2 ppm melamine leavening agent. . After that, the glass sample vial containing 2 ppm: polycyanodin is covered and covered with a lid and shaken up and down to make it fully mixed. The shaking time is about 3 minutes, including 20 zero 111 dimerization. The content of cyanamide leavening agent is about 14~16 bounds (%. • After the melamine test reagent and the sample containing different melamine concentration are prepared), the melamine test reagent is taken in a 2 ml glass dropper and added to the sample a sample. The smelt and the melamine test reagent have a content of 17 to 19 wt% in each sample. Then, the sample vials are respectively capped and shaken up and down 11 201121893 to make the melamine test reagents respectively A sample, B sample and c-like, shaking time is about 3 minutes. Shame, knife this mouth r main r (four) to stand for about 5 minutes to get the upper layer is clarified = two samples and alpha samples. Then, extract A1 Sample, m sample and sample 4 supernatant 'and the quartz quartz colorimetric tube towel. After that, the ultraviolet light _ visible light spectrometer (can be _ wave _ for ~ _ coffee (near chest with different T liquid quartz) Colorimetric tube inspection. Measure ai separately The wavelength absorbance of the product, the sample and the α sample, and use (4) as the blank value sample (secret) at the time of measurement. The experimental results are shown in the "4th drawing" to the "4c drawing", "4th drawing" The sample spectrum of the sample of Α1 (excluding melamine, Cu+NH4C〇3) is used as a standard spectrum because it does not contain melamine; "Fig. 4B" is a sample of m (containing 10 ppm of melamine, Spectral map of Cu+NH4C〇3+melamine); and 4CFig. is a sample spectrum of C1 sample (containing 2 PPm melamine, Cu+NH4C03+melamine). Compare “4A” and “4B” And "C4C", the results show that in the sample spectrum of the B1 sample and the C1 sample, there is a melamine absorption peak in the visible light range of about _瞧 or more (such as "Fig. 4B" and "4C". The figure is not higher than that of the A1 sample containing no melamine (the absorbance at this wavelength is close to 0). Therefore, by comparing "4A" and "4B" and "Picture 4C" can quickly determine whether the sample is determined to contain melamine. Ultraviolet-visible spectrometer can be used for visual inspection. By observing the color change of the mixed solution of the melamine test reagent and the sample, the melamine can be judged whether the sample contains melamine. After the amine test reagent is mixed with the sample, the color conversion between the Ai sample 'm sample and C1« is not obvious (not shown). As shown in Figure 5, the double layer mixture is allowed to stand for about 35 minutes. After that, there is no more than three samples, which are different from the sample and the alpha sample. Therefore, it is immediately known by visual inspection whether the sample contains melamine. Example 2: • *Preparation of the melamine test reagent: The copper sulphate complex was added to the beaker containing acetone for about 3 to 5 minutes until the copper complex was completely dissolved and used. Wherein the content of the copper nitrate complex is about 2 〇~3 〇 wt%. Next, prepare a sample containing different concentrations of melamine: D sample (without melamine): take the melamine-free milk powder and add the glass sample containing the purchased polypropylene to cover the lid and shake it up and down to mix it thoroughly. For 3 to 5 minutes, the content of milk powder containing no melamine is about 14~16 ^ wt.%; E sample (containing 1 〇ppm melamine): adding melamine to the milk powder containing no melamine to prepare l〇ppm Melamine milk powder. After that, the yoghurt milk powder containing chuanchuan is added to the glass sample bottle containing acetone, and then the lid is covered and shaken up and down to make it fully mixed. The shaking time is about 3 to 5 minutes, including 1 〇. The content of ppm melamine milk powder is about 14~16 wt.%; and the sample of F (containing 2 ppm melamine, Cu+NH4C03+melamine): taking 10 ppm of melamine milk powder prepared in sample E, by weight ratio Principle added 13 201121893 Contains no melamine milk powder and makes them fully mixed _ contains a _ tripolyamine milk powder. After that, the 2 ppm melamine milk powder was added to the glass vial containing _, and then the lid was capped and mixed thoroughly by shaking it for about 3 minutes. The t-containing 2PPm tri- melamine milk powder was contained. The content is about 14 to 16% machine. After the preparation of the melamine test reagent and the sample containing different concentrations of trimeramine, 'take the melamine test reagent in 2 ml glass dropper and add it to the d sample, E sample and F sample' to make the melamine test reagent in each sample. It has a content of wt%. At the same time, the addition of the leavening agent to the D sample, the E sample and the F sample respectively made the content of the leavening agent in each sample between 8.5 and 9.5 %, thereby simulating the commercially available milk product. Next, the sample vials were respectively capped, and the dimeric cyanide test reagent was thoroughly mixed with the D sample, the e sample, and the F sample, respectively, and shaken for about 3 minutes. New's stand for about 5 minutes to obtain a supernatant with a clear supernatant and a two-layer mixture of the lower layer of milk powder and leavening agent to form a D1 sample (without melamine 'Cu+NH4C〇3) and E1 samples ( Contains 1 melamine melamine 'ai+NH4C03+melamine) and F1 sample (containing 1 〇ppm melamine,

Cu+NH4C〇3+melamine)。接著,以目視檢測的方式,藉由觀察三 聚氰胺檢驗試劑與樣品混合後的双層混合液之顏色變換,以判斷 樣品中是否含有三聚氰胺。 如「第6A圖」所示,在三聚氰胺檢驗試劑與樣品混合後, D1樣品、E1樣品和Π樣品的顏色變換尚不明顯。如「第6B圖」 所示但疋^這些双層混合液在靜置約35分鐘後,di樣品(不含 三聚氰胺)轉變為紫色,而不同於E1樣品和F1樣品(含有三聚氰 201121893 胺)。因此,可藉由目視檢測的方法立即得知樣品中是否含有三聚 . 氰胺。 實施例3 : 首先’製備三聚氰胺檢驗試劑:將硝酸鈷(c〇balt(n) nifrate hydrate’Co(N〇3)2·χΗ2〇)錯合物加入裝有丙酮之燒杯後攪拌約3〜5 分鐘,至硝酸銅錯合物完全溶解後備用。其中,硝酸銅錯合物之 含買約為2.0〜3.0 wt.%。 φ 接著,製備含有不同三聚氰胺濃度的樣品: G樣品(不含三聚氰胺之膨鬆劑广取不含三聚氰胺之膨鬆劑 (NH4HCO3)加入含有丙酮的玻璃樣品瓶後,蓋上蓋子並以上下搖 動方式使之充份混合,搖動時間約為3〜5分鐘,其巾不含三聚氰 胺之膨鬆劑的含量約為14〜16 wt.% ;以及 Η樣品(含1G綱三聚氰胺):將三聚氰胺加人不含三聚氛胺 之%/#々劑中’配製出含1〇 ppm三聚氰胺膨鬆劑。之後,再將含 _ ppm三聚氰胺膨鬆劑加人含有丙酮的玻璃樣品紐,蓋上蓋子並 以上下搖動方式使之充份混合,搖動時間約為3〜5分鐘,其中含 1〇Ppm二聚氰胺膨鬆劑的含量約為14〜16wt.%。 同樣的在二聚氰胺檢驗試劑和待測定樣品裝備完成後,以2 ㈤玻璃辭抽取三聚氰胺檢驗賴,並添加於G樣品和η樣品 中使一聚氰胺檢驗試劑在各個樣品中具有17〜19 wt.%的含量。 接著,分_樣絲蓋上蓋子,並以上下脑方式使三聚氰胺檢 驗試劑分顺叫品和輯品充似合,搖動日销_分鐘。 15 201121893 然後,靜置約5分鐘以制上層為澄清的上清液以及下層為膨鬆 劑沉澱物的双層混合液,而形成樣品和H1樣品。其中, 樣品為三聚氰胺檢驗試劑與G樣品所形成的双層混合液,而Ηι 樣品則為三聚氰胺檢驗試劑與Η樣品所形成的双層混合液。 接著,分別抽取G樣品、η樣品、G1樣品及Η1樣品的上清 液,並分別裝入石英比色管中。之後,以紫外光_可見光光譜儀(可 掃瞄波長範圍為200〜900 nm(奈米))對裝有不同上清液的石英比色 管進行檢驗。分別測量G樣品、Η樣品、G1樣品及H1樣品的波 長吸收度,並使用丙酮做為測量時的空白值樣品 實驗結果如「第7A圖」至「第7D圖」所示,「第7A圖」為 G樣品(不含三聚氰胺之膨鬆劑,nh^O3)之樣品光譜圖,係做為 對照組,「第7B圖」為Η樣品(含1〇 ppm三聚氰胺^ NH4C〇3+melamine)之樣品光譜圖,係做為對照組;「第7C圖」為 G1樣品(不含三聚氰胺’ 〇>+_〇)3)的樣品光譜圖,在此做為一 標準光譜圖;以及「第7D圖」為H1樣品(含10 ppm三聚氰胺, Co+NH4C03+melamine)的樣品光譜圖。 比較「第7A圖」至「第7D圖」,其結果顯示,在G1樣品的 樣品光譜圖中,於波長約為269 nm的位置具有一非常明顯的特徵 吸收峰(如「第7C圖」所示)。然而,當樣品中含有三聚氣胺時, 如「第7D圖」所示,在H1樣品的樣品光譜圖中,在約3〇5⑽ 的位置出現一二I氣胺吸收峰’而原先位於269 nm的特徵吸收峰 則消失不見。因此,藉由G樣品至H1樣品的樣品光譜圖,可清 201121893 楚的判別樣品中是否具有三聚氰胺的存在。 . 實施例4 : 製備三聚氰胺檢驗試劑:將硝.酸合物加人裝有丙綱之燒 杯錢拌約3〜5分鐘,至俩銘錯合物完全溶解後備用。其中二 硝酸鈷錯合物之含量約為2 〇〜3 〇 wt %。 接著,製備含有不同三聚氰胺濃度的樣品: I樣品(不含三聚驗)··取不含三綠敗奶粉加人含有_ #的玻璃樣品瓶後,蓋上蓋子並以上下搖動方式使之充份混合,搖 動時間約為3〜5分鐘,其中不含三聚氰胺之奶粉的含量約為叫 wt.% ;以及 J樣品(含10PPm三聚氰胺):將三聚氰胺加入不含三聚氛胺之 奶射,配製出含1〇鹏三聚氰胺奶粉。之後,再將含10 ppm 三聚氰胺奶粉加入含有丙_玻璃樣品瓶後,蓋上蓋子並以上下 搖動方式使之充份混合,搖動時_為3〜5分鐘其中含 • 三聚氰胺奶粉(milk+melamine)的含量約為14〜16 wt%。 於三聚氰胺檢驗試劑與含有不同三聚氰胺濃度的樣品配製完 成後,以2 ml玻璃滴管抽取三聚氰胺檢驗試劑,並添加於現品 及J樣品中,使三聚氛胺檢驗試劑在各個樣品中具有口〜η心 • 的含量。接著,分聰樣品瓶蓋上蓋子,並以上下搖動方式使三 聚氰胺檢驗試劑分別與!樣品和j樣品充份混合 分鐘。然後,靜置約5 ~上層輕細上雜 1=層 為奶粉及膨鬆劑沉澱物⑽層混合液,而分卿成^樣品和贝 17 201121893 樣品。 μ然後’分縣n樣品及η樣品的上•,並分職入石英比 色管中。之後,以紫外光-可見光光譜儀(可掃晦波長範圍為2〇〇〜獅 nm(奈抑對財不同上清液的石英比色管進行檢驗。分別測量^ 樣品及II樣品的波長吸收度,並使用_做為測量時的空白值樣 品(blank) 〇 實驗結果如「第8A圖」和「第8B圖」所示,「第8a圖」為 II樣品(不含三聚氰胺,Co+milk)之樣品光譜圖,由於其不含有三 聚氰胺,齡此做為-鮮光譜圖。「第8B圖」為η樣品(含ι〇鹏 三聚氰胺,Co+milk+melamine)之樣品光譜圖,並比較「第圖」 和「第8B圖」。 如「第8B圖」所示’在η樣品的樣品光譜圖中,於波長約 為297nm的位置具有一非常明顯的三聚氰胺吸收峰。因此,可據 此判斷J1樣品中確實具有三聚氰胺。 本發明所揭露之二縣驗驗糊,由於其所 屬錯合物所具有之帶正電較射心軒可與三聚驗之胺基結 σ的特陡。因此’當此三聚氰胺檢驗糊應用於三聚氰胺的檢驗 時’可經由二聚驗檢驗試躺魅變換,或經由料七可見光 光譜儀的制,轉職品巾含有三雜_檢驗絲。由於不 需對所欲檢測的樣品進行如萃取、純化等前處理程序,因此可加 速對樣品的檢驗程序及效率,並大幅降低檢驗樣品時所需耗費的 成本。 201121893 雖然本發明之實施例揭露如上所述,然並作 明,任何熟習相關技藝者,在不脫離本發明之精神限定本發 凡依本發明申請範圍所述之形狀、構造'特徵及精神當二=些= 之變更,因此本發明之專利保護範圍須視本說明書戶斤附之申請專 利範圍所界定者為準。 【圖式簡單說明】 第1圖為本發明之一實施例之檢驗流程示意圖; 鲁 第2圖為本發明之其他實施例之檢驗流程示意圖; 第3圖為本發明之另一實施例之檢驗流程示意圖; 第4A圖至第4C圖為本發明之實施例1之樣品光譜示意圖; 第5圖為本發明之實施例丨之樣品顏色變換示意圖·, 第6A圖和第6B圖為本發明之實施例2之樣品顏色變換不意圖’ 第7A圖至第7D圖為本發明之實施例3之樣品光譜禾意圖,以及 第8A圖和第8B圖為本發明之實施例4之樣品光譜示意圖 【主要元件符號說明】 A1 A1樣品 B1 B1樣品 C1 C1樣品 D1 D1樣品 E1 E1樣品 F1 Π樣品 19Cu+NH4C〇3+melamine). Next, by visually detecting the color change of the two-layer mixture after mixing the melamine test reagent with the sample, it is judged whether or not the sample contains melamine. As shown in Figure 6A, the color change of the D1 sample, the E1 sample, and the ruthenium sample is not significant after the melamine test reagent is mixed with the sample. As shown in Figure 6B, but after the two-layer mixture is allowed to stand for about 35 minutes, the di sample (without melamine) is converted to purple, unlike the E1 sample and the F1 sample (containing the melamine 201121893 amine). ). Therefore, it is immediately known by visual inspection whether the sample contains trimerization. Example 3: First, 'preparation of melamine test reagent: a cobalt nitrate (c〇balt(n) nifrate hydrate'Co(N〇3)2·χΗ2〇) complex was added to a beaker containing acetone and stirred for about 3 to 5 Minutes, until the copper nitrate complex is completely dissolved and ready for use. Among them, the copper nitrate complex contains about 2.0 to 3.0 wt.%. φ Next, prepare samples containing different concentrations of melamine: G sample (without melamine-based leavening agent, take melamine-free leavening agent (NH4HCO3), add it to the glass vial containing acetone, cover it and shake it up and down. Mix it thoroughly, shaking time is about 3~5 minutes, the content of the melamine-free leavening agent is about 14~16 wt.%; and the bismuth sample (including 1G melamine): adding melamine Formulated with 1% by weight of melamine leavening agent in the %/#々剂 containing trimeric amine. After that, add _ppm melamine leavening agent to the glass sample containing acetone, cover and top Shake the mixture to make it fully mixed, the shaking time is about 3~5 minutes, and the content of the 1 pm Ppm melamine leavening agent is about 14~16wt.%. The same in the melamine test reagent and After the measurement sample is completed, the melamine test is extracted with 2 (five) glass words and added to the G sample and the η sample to make the melamine test reagent have a content of 17 to 19 wt.% in each sample. The silk is covered with a lid and The upper and lower brain method allows the melamine test reagent to be mixed with the product and shake the daily sales _ minute. 15 201121893 Then, let stand for about 5 minutes to make the supernatant clear and the lower layer is the leavening agent precipitate. The two-layer mixture forms a sample and a H1 sample, wherein the sample is a two-layer mixture of the melamine test reagent and the G sample, and the Ηι sample is a two-layer mixture of the melamine test reagent and the ruthenium sample. The supernatants of the G sample, the η sample, the G1 sample, and the Η1 sample are respectively taken and loaded into a quartz colorimetric tube. Thereafter, the ultraviolet light-visible spectrometer is used (the scanable wavelength range is 200 to 900 nm (Nai m)) Test the quartz colorimetric tube with different supernatants. Measure the wavelength absorbance of G sample, bismuth sample, G1 sample and H1 sample separately, and use acetone as the blank value sample when measuring. "Picture 7A" to "7D", "Phase 7A" is a sample spectrum of a G sample (without melamine leavening agent, nh^O3), as a control group, "Picture 7B Η samples (including 1) The sample spectrum of 〇ppm melamine^NH4C〇3+melamine) is used as a control group; "Section 7C" is a sample spectrum of G1 sample (without melamine '〇>+_〇)3), here As a standard spectrum; and "7D" is a sample spectrum of the H1 sample (containing 10 ppm melamine, Co+NH4C03+melamine). Comparing "7A" to "7D", the results show that in the sample spectrum of the G1 sample, there is a very characteristic characteristic absorption peak at a position of about 269 nm (such as "7C" Show). However, when the sample contains trimeric gas amine, as shown in the "Fig. 7D", in the sample spectrum of the H1 sample, a dioxin absorption peak at the position of about 3 〇 5 (10) appears and was originally located at 269. The characteristic absorption peak of nm disappears. Therefore, by using the sample spectrum of the G sample to the H1 sample, it is possible to discriminate whether the sample has the presence of melamine in 201121893. Example 4: Preparation of melamine test reagent: The nitrate acid compound was added to a beaker of the genus of the genus, and the mixture was mixed for about 3 to 5 minutes, and the two complexes were completely dissolved and used. The content of the cobalt dichloride complex is about 2 〇~3 〇 wt %. Next, prepare samples containing different concentrations of melamine: I sample (excluding trimerization test) · Take a glass vial containing no green succulent milk powder and containing _ #, cover the lid and shake it up and down to make it Mixing, shaking time is about 3~5 minutes, wherein the content of melamine-free milk powder is about wt.%; and J sample (containing 10PPm melamine): adding melamine to the shot without triethanol, preparing Contains 1 〇 三 melamine milk powder. After that, add 10 ppm melamine milk powder to the bottle containing C-glass, cover it, and mix it by shaking it up and down. When shaking, _ 3~5 minutes containing melamine milk powder (milk+melamine) The content is about 14 to 16 wt%. After the melamine test reagent and the sample containing different melamine concentration are prepared, the melamine test reagent is extracted with a 2 ml glass dropper and added to the current product and the J sample, so that the trimeric amine test reagent has a mouth η in each sample. The content of the heart. Next, cover the lid of the sample bottle, and shake the melamine test reagent separately! The sample and the j sample were mixed thoroughly for a few minutes. Then, let stand for about 5 ~ the upper layer is light and fine, and the 1 = layer is a mixture of milk powder and leavening agent precipitate (10) layer, and is divided into a sample and a sample of 2011 21893. μ then 'sub-count n samples and η samples on the top and separate into the quartz colorimetric tube. After that, the ultraviolet-visible spectrometer (sweepable wavelength range is 2〇〇~lion nm (the quartz colorimetric tube of the different supernatants of Naiyi) is tested. The wavelength absorbance of the sample and the sample II are measured separately. And use _ as the blank value sample (blank) for measurement. The experimental results are shown in "8A" and "8B", and "8a" is II sample (excluding melamine, Co+milk). The sample spectrum, because it does not contain melamine, is the same as the fresh spectrum. "8B" is the sample spectrum of the η sample (containing ι〇鹏 melamine, Co+milk+melamine), and compares the figure And "8B". As shown in "Fig. 8B", in the sample spectrum of the η sample, there is a very obvious melamine absorption peak at a wavelength of about 297 nm. Therefore, the J1 sample can be judged accordingly. There is indeed melamine in the present invention. The second county test paste disclosed in the present invention has a very positive relationship with the amine bond σ of the trimerization test due to the positive charge of the complex compound. When the melamine test paste is applied to the test of melamine The dimerization test is used to test the fascination, or the system of the seven-visible spectrometer is used, and the transfer towel contains three miscellaneous _ test wires. Since it is not necessary to perform pre-treatment procedures such as extraction and purification on the sample to be tested, Accelerating the inspection procedure and efficiency of the sample, and greatly reducing the cost of testing the sample. 201121893 Although the embodiments of the present invention are disclosed above, it will be apparent to those skilled in the art without departing from the invention. The spirit of the present invention is subject to change in the shape, structure 'features and spirits as described in the scope of the application of the present invention. Therefore, the scope of patent protection of the present invention is defined by the scope of the patent application attached to this specification. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view showing a flow of inspection according to an embodiment of the present invention; FIG. 2 is a schematic view showing a flow of inspection according to another embodiment of the present invention; FIG. 3 is another embodiment of the present invention Schematic diagram of the inspection flow; 4A to 4C are schematic diagrams of the sample of the sample of the first embodiment of the present invention; FIG. 5 is a color conversion of the sample of the embodiment of the present invention Intentions, FIG. 6A and FIG. 6B are diagrams showing the sample color conversion of the second embodiment of the present invention. FIGS. 7A to 7D are sample spectra of Example 3 of the present invention, and FIG. 8A and FIG. 8B is a schematic diagram of the spectrum of the sample of Example 4 of the present invention [Description of main components] A1 A1 sample B1 B1 sample C1 C1 sample D1 D1 sample E1 E1 sample F1 Π sample 19

Claims (1)

201121893 七、申請專利範圍·· 1· '一種二聚氣胺檢驗試劑,包含有: 一有機溶劑;以及 -過渡金屬錯合物,溶解於該有機溶财,該過渡金屬錯 合物具有—帶正電之金射心原子,該過渡金屬錯合物係藉由 該帶正電之金射心原子與—三聚氰胺之胺基相結合,而 一過渡金屬化合物。 乂 其中該有機溶劑係選自 其中該過渡金屬錯合物 2.如請求項1所述之三聚氰胺檢驗試劑, 兩酮、乙醇及異丙醇其中之一。 3·如請求項1所述之三聚氰胺檢驗試劑, 係選自硝酸銅或硝酸鈷。 其中該過渡金屬錯合物 4.如請求項1所述之三聚氰胺檢驗試劑, 之重量百分比介於2.0〜3.0之間。 種二聚氰胺之檢驗方法,包括有下列步驟: 提供-三靴驗驗試劑,該三聚氰胺檢驗觸包含 機溶劑及-溶解於該有機溶劑之敬金屬錯合物; 提供一樣品; 混合該二聚氰胺檢驗試劑及該樣品,使形成—混人液· 靜置該混合液,使形成一上清液及一沉毅物; 取該上清液並以一紫外光-可見光光譜儀進行測定,以獲得 一樣品光譜圖;以及 提供一標準光譜圖,並比對該樣品光譜圖與該標準光譜 201121893 圖’以判斷該樣品中是否含有三聚氰胺,若是,則該樣品光譜 • 圖具有—三聚氰胺吸收锋。 6. 如清求項5所述之三聚氰胺之檢驗方法,其中該過渡金屬錯合 物之重量百分比介於2.0〜3 〇之間。 7. 如請求項5所述之三聚氰胺之檢驗方法,其中該有機溶劑係選 自丙酮、乙醇及異丙醇其中之一。 8. 如凊求項5所述之三聚氰胺之檢驗方法,其中該過渡金屬錯合 鲁 物係選自硝酸銅或硝酸鈷。 9. 如清求項8所述之三聚氰胺之檢驗方法,其中該過渡金屬錯合 物係選自硝酸銅,且於靜置該混合液之步驟後,更包括一觀察 該混合液顏色變化之步驟,並依據該混合液判斷該樣品是否具 有該二聚氰胺,若否,則該混合液呈紫色。 10. 如凊求項5所述之三聚氰胺之檢驗方法,其中該樣品係選自膨 鬆劑或奶粉。 如明求項5所述之三聚氰胺之檢驗方法,其中該三聚氰胺檢驗 試劑於該混合液中之重量百分比介於17至19之間。 12.如請求項5所述之三聚氰胺之檢驗方法,其中靜置該混合液之 步驟’係靜置該混合液1至5分鐘。 13 用求項5所述之二聚氰胺之檢驗方法,其巾於靜置該混合液 之步驟前’更包含一搖晃該混合液之步驟。 14·如請求項13所述之三聚驗之檢驗方法,其中該搖晃該混合液 之步驟’係搖晃該混合液1至5分鐘。 21 201121893 15.如請求項5所述之三聚氱胺之檢驗方法,其中於混合該三聚氰 胺檢驗試劑及該樣品之步驟前,更包含提供另一有機溶劑,並 將該樣品與該有機溶劑混合之步驟。201121893 VII. Patent Application Range·· 1· 'A dimeric gas amine test reagent, comprising: an organic solvent; and a transition metal complex dissolved in the organic solvent, the transition metal complex has a band The positively charged gold atomic atom is a transition metal compound by combining the positively charged gold core atom with the amine group of melamine. Wherein the organic solvent is selected from the group consisting of the transition metal complex. 2. The melamine test reagent of claim 1, one of a diketone, ethanol and isopropyl alcohol. 3. The melamine test reagent according to claim 1, which is selected from the group consisting of copper nitrate or cobalt nitrate. Wherein the transition metal complex is 4. The melamine test reagent according to claim 1 is between 2.0 and 3.0. The method for testing melamine comprises the following steps: providing a three-boot test reagent, the melamine test catalyst comprising a solvent and a metal complex dissolved in the organic solvent; providing a sample; mixing the two The melamine test reagent and the sample are allowed to form a mixed liquid, and the mixture is allowed to stand to form a supernatant and a precipitate; the supernatant is taken and measured by an ultraviolet-visible spectrometer to Obtaining a sample spectrum; and providing a standard spectrum and comparing the sample spectrum with the standard spectrum 201121893 to determine whether the sample contains melamine, and if so, the sample spectrum has a melamine absorption front. 6. The method for assaying melamine according to claim 5, wherein the weight percentage of the transition metal complex is between 2.0 and 3 Torr. 7. The method for assaying melamine according to claim 5, wherein the organic solvent is selected from one of acetone, ethanol and isopropyl alcohol. 8. The method for assaying melamine according to claim 5, wherein the transition metal mismatch is selected from the group consisting of copper nitrate or cobalt nitrate. 9. The method for assaying melamine according to claim 8, wherein the transition metal complex is selected from the group consisting of copper nitrate, and after the step of standing the mixture, further comprising the step of observing the color change of the mixture And determining whether the sample has the melamine according to the mixture, and if not, the mixture is purple. 10. The method for assaying melamine according to claim 5, wherein the sample is selected from the group consisting of a bulking agent or a milk powder. The method for assaying melamine according to claim 5, wherein the melamine test reagent is present in the mixture in a weight percentage of between 17 and 19. 12. The method for assaying melamine according to claim 5, wherein the step of allowing the mixture to stand is to leave the mixture for 1 to 5 minutes. 13 The method for testing melamine according to claim 5, wherein the towel comprises a step of shaking the mixture before the step of standing the mixture. 14. The test method of the trimer test described in claim 13, wherein the step of shaking the mixture is to shake the mixture for 1 to 5 minutes. The method for testing a terpene amide according to claim 5, wherein before the step of mixing the melamine test reagent and the sample, further comprising providing another organic solvent, and mixing the sample with the organic solvent The steps. 22twenty two
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CN103163101A (en) * 2013-03-14 2013-06-19 四川大学 Method for fast measuring melamine in milk products
CN103616343A (en) * 2013-12-12 2014-03-05 柴俊沙 Portable melamine detector

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CN106353313B (en) * 2016-11-09 2019-03-29 百奥森(江苏)食品安全科技有限公司 A kind of remaining quick detection kit of melamine in dairy products and application method

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CN101509910B (en) * 2009-03-20 2011-06-22 兰州大学 Reagent and method for rapidly detecting melamine in liquid milk
CN101518825B (en) * 2009-04-07 2011-05-11 华中师范大学 Preparation method of silver nano-particles and application of silver nano-particles to detect melamin

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103163101A (en) * 2013-03-14 2013-06-19 四川大学 Method for fast measuring melamine in milk products
CN103616343A (en) * 2013-12-12 2014-03-05 柴俊沙 Portable melamine detector

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