负离子化学电离GC－MS在单端孢霉烯族毒素分析中的应用

建立了准确、超灵敏的多种单端孢霉烯族毒素的分析方法。方法采用负离子化学电离ＧＣ－ＭＳ技术对十六种单端孢霉烯族毒素的七氟丁酰化衍生物进行气相色谱分离和质谱电离。对每种单端孢霉烯族毒素选择４－５特征碎片离子进行检测，并根据其碎片离子的相对强度和气相色谱保留时间进行鉴定，其检测限可达５×１０（－１１）～０．４×１０（－１２）ｇ。以单离子进行检测，检测限可达１×１０（－１１）～６×１０（－１５）ｇ。该法应用于粮食样品及培养物的测定，检出了以前所建各种方法未曾检出的多种单端抱霉烯族毒素。

Simultaneous and Accurate Analysis of Sixteen Trichothecenes by GC-NICIMS

A ultra-sensitive and accurate gas chromatographic--negative ion chemical ionizationmass spectrometric method(GC-NICIMS) for the simultaneous detection of sixteen trichothecenes in corn and culture has been developed. The method consists of the conversion of the polar trichothecenes into their volatile and stable heptafluoro--butyryl esters,followed by gas chromatographic-mass spectrometric analysis of the derivatives. Thederivatives were ionized under chemical ionization and negative ions were monitored.The samples were screened for the presence of trichothecenes down to I X 10--" to 6 X10(-15)g by monitoring one selected characteristic ion for each analyze. The each detectedcompound was confirmed by monitoring 4 to 5 selected characteristic ions, and comparing their relative intensities and the retention time with that of the standard compound.Picogram (0. 4 -- 50pg) quantities of these trichothecenes could be detected and confirmed, respectively, by this procedure. Several corn and culture samples were analyzedby this method, and several trichothecenes which had not been detected or confirmed before in these samples by other methods were detected.