福建分析测试
福建分析測試
복건분석측시
FUJIAN ANALYSIS & TESTING
2012年
3期
12-17
,共6页
贻贝%固相萃取%液相色谱-串联质谱%大田软海绵酸%鳍藻毒素-1
貽貝%固相萃取%液相色譜-串聯質譜%大田軟海綿痠%鰭藻毒素-1
이패%고상췌취%액상색보-천련질보%대전연해면산%기조독소-1
Mytilus edulis%Solid-Phase Extraction%HPLC-MS/MS%Okadaic acid%Dinophysistoxins-1
采用液相色谱-串联质谱法检测了贻贝中大田软海绵酸（OA）和鳍藻毒素-1（DTX-1）两种腹泻性贝类毒素的含量。样品经80%甲醇水溶液提取,Sep-pak silica固相萃取小柱净化,80%甲醇水溶液定容后供HPLC-MS/MS分析。采用电喷雾负离子模式多反应监测方式进行检测,OA和DTX-1的定量检测的离子对分别为m/z 803.5/255.1和m/z817.4/255.1。2种贝类毒素在20~800μg/L范围内线性良好;在4个添加水平下OA的回收率为79.5%～88.6%,RSD为8.43%～10.4%;DTX-1的回收率为83.8%～91.2%,RSD为4.22%～6.54%。方法灵敏度高,定量限为0.02mg/kg。来自市场和产地的45个贻贝样品残留分析发现,有4个样品检出腹泻性贝类毒素,检出率为8.9%。
採用液相色譜-串聯質譜法檢測瞭貽貝中大田軟海綿痠（OA）和鰭藻毒素-1（DTX-1）兩種腹瀉性貝類毒素的含量。樣品經80%甲醇水溶液提取,Sep-pak silica固相萃取小柱淨化,80%甲醇水溶液定容後供HPLC-MS/MS分析。採用電噴霧負離子模式多反應鑑測方式進行檢測,OA和DTX-1的定量檢測的離子對分彆為m/z 803.5/255.1和m/z817.4/255.1。2種貝類毒素在20~800μg/L範圍內線性良好;在4箇添加水平下OA的迴收率為79.5%～88.6%,RSD為8.43%～10.4%;DTX-1的迴收率為83.8%～91.2%,RSD為4.22%～6.54%。方法靈敏度高,定量限為0.02mg/kg。來自市場和產地的45箇貽貝樣品殘留分析髮現,有4箇樣品檢齣腹瀉性貝類毒素,檢齣率為8.9%。
채용액상색보-천련질보법검측료이패중대전연해면산（OA）화기조독소-1（DTX-1）량충복사성패류독소적함량。양품경80%갑순수용액제취,Sep-pak silica고상췌취소주정화,80%갑순수용액정용후공HPLC-MS/MS분석。채용전분무부리자모식다반응감측방식진행검측,OA화DTX-1적정량검측적리자대분별위m/z 803.5/255.1화m/z817.4/255.1。2충패류독소재20~800μg/L범위내선성량호;재4개첨가수평하OA적회수솔위79.5%～88.6%,RSD위8.43%～10.4%;DTX-1적회수솔위83.8%～91.2%,RSD위4.22%～6.54%。방법령민도고,정량한위0.02mg/kg。래자시장화산지적45개이패양품잔류분석발현,유4개양품검출복사성패류독소,검출솔위8.9%。
Establish the detection method of okadaic acid（OA） and dinophysistoxins（DTX-1） in Mytilus edulis using high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）.Shellfish sample was extracted by 80% methyl.Shellfish extract solution was clean-up by Sep-pak silica column.A triple-quadrupole tandem mass spectrometer was used as a detector for HPLC to determine OA.As for the MS/MS,the multi-reactions monitoring（MRM） scan type and the negative ion electrospray ionization（-ESI） mode were applied.The precursor ion→product ion（m/z 803.5→m/z 255.1,m/z 803.5→m/z 563.1） was selected as OA quantitate detection ion pair.The precursor ion→product ion（m/z 817.4→m/z 255.1,m/z 817.4→m/z 113.1） was selected as DTX-1 quantitate detection ion pair.The mobile phase of HPLC was the methyl cyanide： 1% methanoic acid-water（vol/vol： 70：30） and the chromatographic column was Zorbax XDB-C18（2.1mm×150mm×5μm）.The standard OA and DTX-1,the shellfish being added with OA and DTX-1,the shellfish sample were determine by the HPLC-MS/MS.The standard curve for OA showed good linearity over the concentration range of 5~640 ng/ml,the equation of linear regression was Y =207X-241（Q1/Q3：m/z 803.5→255.1）,r was 0.9998,The recovery of sample being added with OA was 79.5%～88.6% and the RSD was 8.43%～10.4%.The standard curve for DTX-1 showed good linearity over the concentration range of 0 ~ 200 ng/ml,the equation of linear regression was Y =141X ＋3.59×103（Q1 /Q3： m / z817.4→255.1）,r was 0.9997,The recovery of sample being added with DTX-1 was83.8%～91.2% and the RSD was 4.22%～6.54%.This HPLC-MS/MS is highly sensitive,fast,and very accurate.So it can be used for detecting the remain of OA and its natural derivative DTX-1 in shellfish.Among the 45 samples from the origin and market,4 samples were detected DSP,the ratio was 8.9%.
