液相色譜-串聯質譜法測定豬尿液中地西泮及其7種(zhǒng)代謝物殘留

2021-03-16 11:02:58 田永清,廖夏露,鄭明學(xué),等 2021年第3《中國(guó)什章動物檢疫》

爲建立快速測定豬尿中地西泮及其7種(zhǒng)代謝物殘留的超高效喝不液相色譜-串聯質譜(UPLC-MS/MS)确證森子方法,本研究優化了樣(yàng)品淨化的陽離子交換固相萃取柱(PC高弟X柱)及其淋洗洗脫條件。豬尿液酸化後(hòu)直短懂接經(jīng)PCX柱淨化,依國歌次用水、60%甲醇水溶液淋洗,最後(hòu)用5%氨化甲醇洗脫;選技房用BEH C18色譜柱分離,UP也音LC-MS/MS進(jìn)行檢測站市,以基質匹配标準曲線定量。結果顯示:長刀8種(zhǒng)藥物在0.3~20.0 μg綠微/L範圍内具有良好(hǎo)的線性關系(R2≥0.99術了5),檢出限和定量限分别爲0.1 μg/L和0.3 μg/L;各藥物在3個添那她加濃度下回收率爲73.6%~95.3%,日内、日間相對(車頻duì)标準偏差分别爲2.9%~18.6%(n=6子亮)和2.2%~12.6%(n=3)。內文結果表明,本方法操作簡單、快速,靈敏度高、特異性好(h什金ǎo)。

Determination of Diazepam an商現d Its Metabolite Resid窗醫ues

in Swine Urine by UPLC-MS/MS

In order to establish an ultra現數 performance liqui山問d chromatography-tandem mass s懂拿pectrometry(UPLC-MS/M一玩S)to determine diazepam and下和 its seven metabolite re匠銀sidues(temazepam,nimetazepam,兵來nordiazepam,oxaze金機pam,nitrazepam,7-amin從自onitrazepam and 7-aminonimetazepam)i討制n swine urine,a cation exchange高房 solid phase extraction column船很(PCX column)and i鐵開ts conditions of eluti秒科on were optimized. Swine urine wa現舞s directly purified by P吃他CX column after being acidized,多靜washed with water and 60% methanol 理黃water solution i木麗n turn,and then eluted with 5% 低內ammoniated methanol;河輛then the pre-treated urine可書 sample was separated by B動跳EH C18 column,d土什etected by UPLC-MS/MS,and q問女uantified by matrix-matched external st書器andard curves. The results店爸 showed that a good linear relat下你ionship(R2≥0.995)among t動習he eight drugs was輛錢 obtained within 0.你人3 to 20 μg/L,the l在公imits of detecti討快on and quantification were 0.1 and 0.車雜3 μg/L respecti靜輛vely;the mean recover算說ies varied from 73.6%遠煙 to 95.3% at the t笑自hree concentrations,the rel美們ative standard de長國viations of intra睡體 and inter day were 2.9% to 18.6%(n=動費6)and 2.2% to 12.6%(n=3),respectively. 術信It was concluded that the propo村紙sed method was simple and rapid wit路從h high sensitivity and specificity.

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