食品安全质量检测学报
食品安全質量檢測學報
식품안전질량검측학보
Journal of Food Safety & Quality
2015年
9期
3677-3683
,共7页
磺酸化磁珠%磁固相萃取法%液相色谱-串联质谱法%苯二氮卓类物质%牛肉
磺痠化磁珠%磁固相萃取法%液相色譜-串聯質譜法%苯二氮卓類物質%牛肉
광산화자주%자고상췌취법%액상색보-천련질보법%분이담탁류물질%우육
sulfo-functionalized magnetic beads%magnetic solid phase extraction%liquid chromatography-tandem mass spectrometry%benzodiazepines%beef
目的：以磺酸化磁珠作为磁固相萃取吸附剂,建立了磁固相萃取-液相色谱-串联质谱法联用分析苯二氮卓类药物的新方法。方法萃取和吸附条件优化后,地西泮、奥沙西泮、三唑仑和氯氮卓4种苯二氮卓类药物经磺酸化磁珠富集后,采用液相色谱-串联质谱的多反应方法检测牛肉样品中4种苯二氮卓类药物的残留。结果4种苯二氮卓类药物的方法回收率为49.6%~83.5%,相对标准偏差(RSD, n=5)为2.2%~16.0%,检出限范围为0.13~0.79 ng/mL,定量限范围为0.44~2.63 ng/mL,在1.0~25.0μg/L 范围内线性相关系数为0.9992~0.9999。结论该法具有操作简便、灵敏度高、测定准确等特点,适用于牛肉中苯二氮卓类物质的残留检测。
目的：以磺痠化磁珠作為磁固相萃取吸附劑,建立瞭磁固相萃取-液相色譜-串聯質譜法聯用分析苯二氮卓類藥物的新方法。方法萃取和吸附條件優化後,地西泮、奧沙西泮、三唑崙和氯氮卓4種苯二氮卓類藥物經磺痠化磁珠富集後,採用液相色譜-串聯質譜的多反應方法檢測牛肉樣品中4種苯二氮卓類藥物的殘留。結果4種苯二氮卓類藥物的方法迴收率為49.6%~83.5%,相對標準偏差(RSD, n=5)為2.2%~16.0%,檢齣限範圍為0.13~0.79 ng/mL,定量限範圍為0.44~2.63 ng/mL,在1.0~25.0μg/L 範圍內線性相關繫數為0.9992~0.9999。結論該法具有操作簡便、靈敏度高、測定準確等特點,適用于牛肉中苯二氮卓類物質的殘留檢測。
목적：이광산화자주작위자고상췌취흡부제,건립료자고상췌취-액상색보-천련질보법련용분석분이담탁류약물적신방법。방법췌취화흡부조건우화후,지서반、오사서반、삼서륜화록담탁4충분이담탁류약물경광산화자주부집후,채용액상색보-천련질보적다반응방법검측우육양품중4충분이담탁류약물적잔류。결과4충분이담탁류약물적방법회수솔위49.6%~83.5%,상대표준편차(RSD, n=5)위2.2%~16.0%,검출한범위위0.13~0.79 ng/mL,정량한범위위0.44~2.63 ng/mL,재1.0~25.0μg/L 범위내선성상관계수위0.9992~0.9999。결론해법구유조작간편、령민도고、측정준학등특점,괄용우우육중분이담탁류물질적잔류검측。
Objective To establish a novel method for the determination of 4 kinds of benzodiazepines (BZDs, chlordiazepoxide, diazepam, oxazepam, and triazolam) by magnetic solid phase extraction (MSPE)-liquid chromatography-tandem mass spectrometry (LC-MS/MS), based on the sulfo-functionalized magnetic beads. Methods After optimization of the extraction/desorption conditions, 4 BZDs were extracted with sulfo-functionalized magnetic beads, and detected by liquid chromatography-tandem mass spectrometry in multiple-reaction monitoring mode. Results The average recoveries of 4 benzodiazepines were 49.6%~83.5%, the relative standard deviation (RSD) of this method was between 2.2%~16.0%. The limits of detection (LOD) and limits of quantification (LOQ) of 4 kinds of benzodiazepines were in the range of 0.13~0.79 and 0.44~2.63 ng/mL, respectively. This method had a good linearity in the range of 1.0~25.0μg/L between the peak areas and concentration in 4 kinds of benzodiazepines with the correlation coefficients were 0. 9992~0.999. Conclusion The method was fast, accurate and sensitive, which could be applied in the routine assay on benzodiazepines in beef.
