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HPLCMS/MS法检测中华鳖中磺胺类药物残留[J]. 水生生物学报, 2008, 32(5): 669-679.
引用本文: HPLCMS/MS法检测中华鳖中磺胺类药物残留[J]. 水生生物学报, 2008, 32(5): 669-679.
ZHANG Yong-Zheng, XU Xiao-Lin, ZHANG Hai-Qi, FANG Mei-Juan, PAN Li-Xin, LU Hong-Fa. SIMULTANEOUS DETERM INATION OF TWENTY ONE SULFONAMIDE RESIDUES IN TRION YX SINENSIS BY HIGH PERFORMANCE L IQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY[J]. ACTA HYDROBIOLOGICA SINICA, 2008, 32(5): 669-679.
Citation: ZHANG Yong-Zheng, XU Xiao-Lin, ZHANG Hai-Qi, FANG Mei-Juan, PAN Li-Xin, LU Hong-Fa. SIMULTANEOUS DETERM INATION OF TWENTY ONE SULFONAMIDE RESIDUES IN TRION YX SINENSIS BY HIGH PERFORMANCE L IQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY[J]. ACTA HYDROBIOLOGICA SINICA, 2008, 32(5): 669-679.

HPLCMS/MS法检测中华鳖中磺胺类药物残留

SIMULTANEOUS DETERM INATION OF TWENTY ONE SULFONAMIDE RESIDUES IN TRION YX SINENSIS BY HIGH PERFORMANCE L IQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY

  • 摘要: 建立了一种液相色谱-电喷雾串联质谱同时测定中华鳖中21种磺胺类药物残留的方法。均质样品先后用乙腈、二氯甲烷提取,合并提取液,取部分提取液经氮吹浓缩。残渣用1mL流动相溶解,饱和正己烷脱脂净化。采用ZORBAX Ec lipse XDB-C8色谱柱,以含0.2%乙酸的水溶液和甲醇(7∶3)为流动相,梯度洗脱,在电喷雾-多反应监测离子模式下,进行定量定性分析。方法的定量限为4μg/kg;以标准加入法计算回收率,在4—40μg/kg添加范围内,平均回收率为75.2%—104%;相对标准偏差为0.16%—9.98%。

     

    Abstract: Sulfonam ides are widely used in fisheries for prevention of d iseases.W ith the public. sincreasing concern withthe food safety, residues of sulfonam ides infishery products should arouse regards.Improper use or miproper withdraw tmiewill lead to the presence of sulfonam ide residues in fishery products, which can influence human food security and polluteenvironment possibly.M any countries have established the maxmium allowable residue lmiits for sulfonam ides in fisheryproducts1T herefore, it is necessary to establish the analys is method for the detection of sulfonamides residues in fisheryproducts.A method of smi ultaneous determ ination of twenty-one commonly used sulfonam ideresidues inTrionyx sinensis by high performance liquid chromatography-electro spray tandem mass spectrometry (HPLC /MS /MS) is described.Sulfonamide residues were extracted from hom ogenized tissue with aceton itrile and dichlorom ethane.A part of theextract was taken and then dried by n itrogen.The residue were dissolved into 1mL mobile phase and defatted w ith n-hexane( saturated by acetonitrile) 1T he 21 analytes w ere separated on ZORBAX EclipseXDB-C8 Column w ith mobile phasescontainingm ethanol and 012% acet ic acid and finally determ ined by electrospray ion ization tandem m ass spectrometry( ESI-MS-MS).A linear gradient eluting programo fmethanol from 30% to 80%(V /V)was employed at a flow rate of 012mL /m in in 35m inutes1Ana lytes confirmation were perform ed usingm ultiple reaction monitoring (MRM) with one precursorionand two productions as identifiers1T he quantitative lmi it of method was 4Lg /kg1Recoveries tested by standardaddition method were in the range of 7512% )104%, RSDs were in the range of0116% ) 9198% at a spiking level from4Lg /kg to 40Lg /kg(n= 6).

     

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