大田软海绵酸液相色谱串联质谱检测方法的研究  

Study on okadaic acid in shellfish using high performance liquid chromatography with triple-quadrupole tandem mass spectrometry

作　　者：卢士英[1] 张代辉[2] 周玉[1] 任洪林[1] 孟宪梅[1] 柳增善[1] 于光 

机构地区：[1]吉林大学教育部人兽共患病重点实验室,长春130062 [2]吉林进出口检验检疫局,长春130062

出　　处：《中国卫生检验杂志》2007年第9期1537-1539,1551,共4页Chinese Journal of Health Laboratory Technology

基　　金：国家质检总局资助项目(2003IK044);国家自然基金资助项目(30671762)

摘　　要：目的：利用高效液相色谱一串联质谱法建立海产品中大田软海绵酸（Okadaic acid，OA）的检测方法。方法：贝样品提取液经AccuBond^Ⅱ SPE silica固相萃取小柱预分离和富集，用三级四极杆串联质谱（MS／MS）作为HPLC的检测器，使用正离子电喷雾（ESI）电离方式，多反应监测（MRM）扫描模式，选择母一子离子对m／z 827→m／z723，m／z827→m／z809作为定量检测的离子对，HPLC的流动相为乙腈：1％甲酸-水（体积比70：30），色谱柱为Agilent Extend—C18（2．1×150mm，φ5．0μm），对OA标准品及加标样品和实际样品进行HPLC—MS／MS检测。结果：方法线性回归方程为Y=193．07X-780．6（Q1／Q3：m／z827．4→723．5）；Y=83．021X-335．6（Q1／Q3：m／z827．4→809．5），相关系数一均为0．9991；线性范围为10～800μg／L。样品平均回收率为83．99％，平均RSD为4．34％。结论：建立的HPLC—MS／MS方法灵敏、快速、准确．可用于海产品中贝类样品OA限量标准检测。Objective：To establish the detection method of okadaic acid（OA） in shellfish using high performance liquid chromatography- tandem mass spectrometry. Methods：Shellfish extract was preseparated and gathered by AccuBond^Ⅱ SPE silica column extractor. 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 positive ion electrospray ionization （ ESI ） mode were employed. The precursor ion→product ion （m/z 827→ m/z 723, m/z 827→m/z 809 ） was selected as 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 the agilent extend -C18（2. 1 × 150 ram, 05.0 μm）. The standard OA, the shellfish being added with OA and the shellfish sample were determine by the HPLC - MS/MS. Results：The standard curve for OA showed good linearity over the concentration range of 10 - 800 ng/ml, the equation of linear regression was Y = 193.07X -780. 6 （ Q1/Q3 ： m/z 827.4→723. 5 ） ; Y = 83. 021X - 335.6（ Q1/Q3 ： m/z 827.4→809.5 ） ,r^2 were all 0. 9991, The average recovery of sample being added with OA was 83.99% and the average RSD was 4. 34%. Conclusion：This HPLC - MS/MS is highly sensitive, fast, and very accurate. So it can be used for detecting limit of OA in shellfish.

关 键 词：大田软海绵酸 高效液相色谱-串联质谱法 固相萃取 贝 

分 类 号：O657.63[理学—分析化学]