分析试验室
分析試驗室
분석시험실
ANALYTICAL LABORATORY
2010年
3期
23-26
,共4页
刘承兰%钟国华%胡美英%罗建军%郝卫宁
劉承蘭%鐘國華%鬍美英%囉建軍%郝衛寧
류승란%종국화%호미영%라건군%학위저
气相色谱-质谱联用%同位素稀释%茶叶%杀菌剂
氣相色譜-質譜聯用%同位素稀釋%茶葉%殺菌劑
기상색보-질보련용%동위소희석%다협%살균제
Gas chromatography-mass spectrometry%Isotopic dilution%Tea%Fungicides
建立了使用固相萃取-气相色谱/质谱联用结合同位素稀释技术准确测定3种茶叶(红茶、绿茶和普洱茶)中敌菌丹、克菌丹、灭菌丹、百菌清和苯氟磺胺等杀菌剂农药残留的新方法. 茶叶试样中加入同位素内标D6-克菌丹,经乙腈匀浆提取,提取液离心后取上清液经Forisil固相萃取柱浓缩、净化. GC-MS采用选择离子监测(SIM)模式进行定性定量分析,内标法定量. 方法的添加回收率为74.1%~100.6%;相对标准偏差为1.2%~12%;6种农药的检出限为0.002~0.14 μg/mL.
建立瞭使用固相萃取-氣相色譜/質譜聯用結閤同位素稀釋技術準確測定3種茶葉(紅茶、綠茶和普洱茶)中敵菌丹、剋菌丹、滅菌丹、百菌清和苯氟磺胺等殺菌劑農藥殘留的新方法. 茶葉試樣中加入同位素內標D6-剋菌丹,經乙腈勻漿提取,提取液離心後取上清液經Forisil固相萃取柱濃縮、淨化. GC-MS採用選擇離子鑑測(SIM)模式進行定性定量分析,內標法定量. 方法的添加迴收率為74.1%~100.6%;相對標準偏差為1.2%~12%;6種農藥的檢齣限為0.002~0.14 μg/mL.
건립료사용고상췌취-기상색보/질보련용결합동위소희석기술준학측정3충다협(홍다、록다화보이다)중활균단、극균단、멸균단、백균청화분불광알등살균제농약잔류적신방법. 다협시양중가입동위소내표D6-극균단,경을정균장제취,제취액리심후취상청액경Forisil고상췌취주농축、정화. GC-MS채용선택리자감측(SIM)모식진행정성정량분석,내표법정량. 방법적첨가회수솔위74.1%~100.6%;상대표준편차위1.2%~12%;6충농약적검출한위0.002~0.14 μg/mL.
A new method using isotopic dilution and solid phase extraction (SPE) technique was established to determine the residues of captafol, captan, folpet, chlorothalonil, and dichlofluanid in three kinds of tea (red tea, green tea and Pu'er) by gas chromatography-mass spectrometry (GC-MS). Isotope internal standard, D6-captan was added into tea leaves, and the sample was extracted by acetonitrile and cleaned up by solid phase extraction using Florisil sorbent. The mass spectrometer was operated with selected ion monitoring (SIM) mode. The target analytes were quantified by isotope internal standard method. Average recoveries ranged from 74.1% to 100.6% and relative standard deviations were 1.2%~11% at six fortified levels. Detection limits of five fungicides were 0.002~0.14 μg/mL.The proposed method is characterized by simplicity, high sensitivity and accuracy.