頂空—?dú)庀嗌V法測定茶葉中三氯殺螨醇?xì)埩袅康难芯?/title> <meta name="keywords" content="色譜,茶葉,氣相,殘留量,法測定"> <meta name="description" content="摘要：該文提出頂空進(jìn)樣-氣相色譜外標(biāo)法快速測定茶葉中三氯殺螨醇的定量方法。樣品中的三氯殺螨醇在乙醇-氫氧化鉀介質(zhì)下，分解為雙（對氯苯基）-甲酮（DBP）和三氯甲烷，用帶有電子捕獲檢測器的氣相色譜儀檢測三氯甲烷。結(jié)果表明，在給定濃度范圍內(nèi)，三氯甲烷的質(zhì)量濃度與峰面積呈良好線性關(guān)系，樣品的加標(biāo)回收率在7"> <meta http-equiv="Content-Type" content="text/html; charset=gb2312" /> <meta http-equiv="Cache-Control" content="no-transform" /> <meta http-equiv="Cache-Control" content="no-siteapp" /> <link href="/css/head.css" rel="stylesheet" type="text/css" /> <link href="/css/news.css" rel="stylesheet" type="text/css" /> <link href="/css/foot.css" rel="stylesheet" type="text/css" /> <link href="/css/xin.css" rel="stylesheet" media="screen" type="text/css"> <script type="text/javascript" src="http://www.zuancaijixie.com/statics/js/jquery.min.js"></script> <script type="text/javascript" src="http://www.zuancaijixie.com/statics/js/jquery.sgallery.js"></script> <script 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class="det_content" id="zoom"> <p><script type="text/javascript">ok3w_ads("s004");</script></p> <div id="urg1j081" class=ggad><script type="text/javascript">ok3w_ads("s005");</script></div> <img src="http://img1.qikan.com.cn/qkimages/zspy/zspy201412/zspy20141223-1-l.JPG" alt="http://img1.qikan.com.cn/qkimages/zspy/zspy201412/zspy20141223-1-l.JPG" /><img src="http://img1.qikan.com.cn/qkimages/zspy/zspy201412/zspy20141223-2-l.JPG" alt="http://img1.qikan.com.cn/qkimages/zspy/zspy201412/zspy20141223-2-l.JPG" /> <br>　　摘要：該文提出頂空進(jìn)樣-氣相色譜外標(biāo)法快速測定茶葉中三氯殺螨醇的定量方法。樣品中的三氯殺螨醇在乙醇-氫氧化鉀介質(zhì)下，分解為雙（對氯苯基）-甲酮（DBP）和三氯甲烷，用帶有電子捕獲檢測器的氣相色譜儀檢測三氯甲烷。結(jié)果表明，在給定濃度范圍內(nèi)，三氯甲烷的質(zhì)量濃度與峰面積呈良好線性關(guān)系，樣品的加標(biāo)回收率在71.1%～94.9%之間，相對標(biāo)準(zhǔn)偏差小于2.6%。該方法準(zhǔn)確、簡便、快速，能滿足茶葉中三氯殺螨醇的檢測需要。<br>　　關(guān)鍵詞：頂空氣相色譜茶葉三氯殺螨醇堿解反應(yīng)<br>　　中圖分類號：R155 文獻(xiàn)標(biāo)識碼：A 文章編號：1672-5336（2014）24-0000-00<br>　　三氯殺螨醇又稱開樂散，是一種有機(jī)氯殺螨劑。對螨類有觸殺和胃毒作用，對成螨、幼螨及卵均有效�；瘜W(xué)性質(zhì)穩(wěn)定，在自然條件下不易降解，該藥施藥1年后作物仍有少量殘留[1]。三氯殺螨醇的檢測，早期有比色法、薄層法和紫外光譜法，近年來多采用氣相色譜法[2]和液相色譜法[3]，但這些檢測方法樣品的前處理過程較繁瑣，誤差較大，試劑消耗量大。本文所采用的頂空-氣相色譜法的原理是：三氯殺螨醇在堿性條件下能水解成二氯苯酮和氯仿[4]。其反應(yīng)方程式為：<br>　　1 實(shí)驗(yàn)部分<br>　　1.1 儀器和試劑<br>　　氣相色譜儀（GC）：7890A，帶ECD檢測器，Agilent Technologies；<br>　　頂空自動進(jìn)樣器：CTC analytic，Agilent Technologies；<br>　　電子天平：ML204，Mettler Toledo 公司；氫氧化鈉：（優(yōu)級純）；<br>　　三氯殺螨醇：100μg/mL，農(nóng)業(yè)部環(huán)境保護(hù)科研監(jiān)測所研制；<br>　　無水乙醇（分析純）；<br>　　石油醚（分析純）；<br>　　1.2 色譜條件及頂空進(jìn)樣條件<br>　　色譜柱：HP-5 毛細(xì)管柱（30 m×0.32 mm×0.25 μm）；<br>　　進(jìn)樣口溫度：220 ℃；檢測器溫度：300 ℃；<br>　　載氣流量：N2 1.0 mL/ L；進(jìn)樣量：1 mL；<br>　　尾吹流量：25 mL/ L；分流比：20：1；<br>　　柱溫：初溫 35℃，保持5min，繼續(xù)以15 ℃ /min 的速率升溫到 80 ℃，最后以 40 ℃ /min 的升溫到230 ℃，保持5min；<br>　　頂空溫度：55 ℃；樣品頂空平衡時(shí)間：30 min；進(jìn)樣針溫度：60℃。<br>　　1.3 溶液配制<br>　�。�1）標(biāo)準(zhǔn)品儲備液：將三氯殺螨醇用正己烷配制成濃度為10μg/mL 的溶液，于 4℃保存。<br>　　（2）氫氧化鈉儲備液：現(xiàn)配10mol/L的氫氧化鈉溶液[5]。<br>　　1.4 樣品制備<br>　　稱取0.1000 g 樣品（準(zhǔn)確到0.0001 g）于20mL頂空瓶中，先用0.5mL石油醚30℃振搖提取30min。再依次加入0.5mL無水乙醇和5mL 10mol/L的氫氧化鈉溶液，充分混勻，使其進(jìn)行堿解反應(yīng)，頂空進(jìn)樣。<br>　　1.5 標(biāo)準(zhǔn)曲線的配制<br>　　分別稱取0.1000 g 不含三氯殺滿醇的茶葉（準(zhǔn)確到0.0001 g）于6個(gè)20mL頂空瓶中，<br>　　依次加入0.00μg，0.01μg，0.05μg，0.10μg，0.50μg，1.00μg三氯殺螨醇標(biāo)準(zhǔn)品[7]，再加入0.5mL無水乙醇和5mL10mol/L的氫氧化鈉溶液，渦旋振動器上震動5min充分混勻，使其進(jìn)行堿解反應(yīng)，直接頂空進(jìn)樣。<br>　　1.6 測定<br>　　按 1.2 條件，以目標(biāo)物三氯甲烷的保留時(shí)間為定性依據(jù)，三氯甲烷溶液的濃度為<br>　　橫坐標(biāo)，峰面積為縱坐標(biāo)，作線性回歸方程，根據(jù)標(biāo)準(zhǔn)曲線外標(biāo)法定量。三氯甲烷的出峰時(shí)間大致為4.095 min 左右，其譜圖見圖 1。<br>　　圖1 三氯殺螨醇含量為 0.10μg 色譜圖<br>　　2 結(jié)果與討論<br>　　2.1 樣品前處理方法的選擇<br>　　本方法涉及的前處理最主要的是提取和堿解反應(yīng)。稱取0.1000 g 含三氯殺滿醇的<br>　　茶葉（準(zhǔn)確到0.0001 g），先用0.5mL石油醚提取，分別振搖10min，30min，60min，90min，120min，在相同條件下進(jìn)行頂空進(jìn)樣，外標(biāo)法定量，結(jié)果表明30min振搖后，測得的值最高，其譜圖見圖2；用石油醚提取后，室溫下[5]，再加入5mL10mol/L的氫氧化鈉溶液進(jìn)行堿化反應(yīng)，分別采取充分振搖10 min，20min，30min后頂空分析和充分混勻后直接頂空分析，結(jié)果表明兩種方式的結(jié)果無顯著差異。因此最終選用充分混勻后直接頂空分析。<br>　　圖2 振搖時(shí)間對三氯殺螨醇提取率的影響<br>　　2.2 頂空進(jìn)樣條件的選擇<br>　　因?yàn)镋CD檢測器檢測的物質(zhì)是三氯甲烷，因此，選用已成熟的三氯甲烷的頂空及色<br>　　譜條件。但考慮到溫浴對堿化反應(yīng)的平衡移動的影響，平衡時(shí)間分別選擇30 min，60 min，90 min；平衡溫度分別選擇40℃，55℃，60℃。<br>　　表1 頂空進(jìn)樣器參數(shù)設(shè)置值<br>　　儀器參數(shù)設(shè)置值/min<br>　　溫浴40℃溫浴55℃溫浴55℃溫浴55℃溫浴60℃<br>　　樣品瓶平衡時(shí)間30 min30 min30 min60 min30 min<br>　　試驗(yàn)結(jié)果表明，平衡時(shí)間同為30min，溫浴溫度為55℃時(shí)，所測得的結(jié)果達(dá)到最大<br>　　值；溫浴55℃，平衡時(shí)間30min～90min，結(jié)果無顯著差異。因此，最終確定的最佳參數(shù)值見“1.2 色譜條件及頂空進(jìn)樣條件”。<br>　　2.3 方法考察<br>　　2.3.1 標(biāo)準(zhǔn)曲線和檢出限、定量限<p style="margin-bottom:10px"><strong>相關(guān)熱詞搜索：</strong><a href="http://www.zuancaijixie.com/tag/%C9%AB%C6%D7.html" target="_blank">色譜</a> <a href="http://www.zuancaijixie.com/tag/%B2%E8%D2%B6.html" target="_blank">茶葉</a> <a href="http://www.zuancaijixie.com/tag/%C6%F8%CF%E0.html" target="_blank">氣相</a> <a 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