色谱
色譜
색보
Chinese Journal of Chromatography
2015年
11期
1199-1204
,共6页
木合他拜尔%严华%徐姗%冯楠%郝杰%朱尘琪%郭爽%张朝晖%韩南银
木閤他拜爾%嚴華%徐姍%馮楠%郝傑%硃塵琪%郭爽%張朝暉%韓南銀
목합타배이%엄화%서산%풍남%학걸%주진기%곽상%장조휘%한남은
QuEChERS%超高效液相色谱-高分辨串联质谱%抗球虫药%鸡肉
QuEChERS%超高效液相色譜-高分辨串聯質譜%抗毬蟲藥%鷄肉
QuEChERS%초고효액상색보-고분변천련질보%항구충약%계육
QuEChERS%ultra high liquid chromatography-high resolution mass spectrometry%anticoccidials%chicken
建立了鸡肉中二硝托胺、尼卡巴嗪、地克珠利、妥曲珠利、莫能菌素及盐霉素6种抗球虫药物的超高效液相色谱-高分辨串联质谱多残留检测方法。经 QuEChERS样品净化,首先使用含有1%( v/v)三氯乙酸的乙腈-水(3:7, v/v)溶液提取样品中的被测物,再加入氯化钠,使用50 mg/mL N-丙基乙二胺( PSA)+50 mg/mL 中性氧化铝( Alumina-N)的混合分散固相萃取( dispersive solid phase extraction,DSPE)粉末净化提取,过0.22μm 滤膜后以超高效液相色谱-高分辨串联质谱检测。选择 Waters Acquity UPLC? BEH C8色谱柱(100 mm×2.1 mm,1.7μm),以甲醇-5 mmol/L醋酸铵水溶液为流动相进行梯度洗脱。使用正、负离子同时扫描模式,基质外标法定量。研究表明,6种目标化合物的线性范围为:二硝托胺,1.0~30.0μg/L;尼卡巴嗪,0.2~6.0μg/L;地克珠利、妥曲珠利,2.0~60.0μg/L;莫能菌素、盐霉素,4.0~120.0μg/L。空白样品中添加低、中、高3个水平的混合标准溶液,回收率在67.7%~126.8%之间,相对标准偏差( RSD )≤10.4%。6种抗球虫药物的定量限分别为:二硝托胺,2.50μg/kg;尼卡巴嗪,0.50μg/kg;地克珠利、妥曲珠利,5.00μg/kg;莫能菌素、盐霉素,20.00μg/kg。该方法操作简便,灵敏度高,且能够满足日常检测要求。
建立瞭鷄肉中二硝託胺、尼卡巴嗪、地剋珠利、妥麯珠利、莫能菌素及鹽黴素6種抗毬蟲藥物的超高效液相色譜-高分辨串聯質譜多殘留檢測方法。經 QuEChERS樣品淨化,首先使用含有1%( v/v)三氯乙痠的乙腈-水(3:7, v/v)溶液提取樣品中的被測物,再加入氯化鈉,使用50 mg/mL N-丙基乙二胺( PSA)+50 mg/mL 中性氧化鋁( Alumina-N)的混閤分散固相萃取( dispersive solid phase extraction,DSPE)粉末淨化提取,過0.22μm 濾膜後以超高效液相色譜-高分辨串聯質譜檢測。選擇 Waters Acquity UPLC? BEH C8色譜柱(100 mm×2.1 mm,1.7μm),以甲醇-5 mmol/L醋痠銨水溶液為流動相進行梯度洗脫。使用正、負離子同時掃描模式,基質外標法定量。研究錶明,6種目標化閤物的線性範圍為:二硝託胺,1.0~30.0μg/L;尼卡巴嗪,0.2~6.0μg/L;地剋珠利、妥麯珠利,2.0~60.0μg/L;莫能菌素、鹽黴素,4.0~120.0μg/L。空白樣品中添加低、中、高3箇水平的混閤標準溶液,迴收率在67.7%~126.8%之間,相對標準偏差( RSD )≤10.4%。6種抗毬蟲藥物的定量限分彆為:二硝託胺,2.50μg/kg;尼卡巴嗪,0.50μg/kg;地剋珠利、妥麯珠利,5.00μg/kg;莫能菌素、鹽黴素,20.00μg/kg。該方法操作簡便,靈敏度高,且能夠滿足日常檢測要求。
건립료계육중이초탁알、니잡파진、지극주리、타곡주리、막능균소급염매소6충항구충약물적초고효액상색보-고분변천련질보다잔류검측방법。경 QuEChERS양품정화,수선사용함유1%( v/v)삼록을산적을정-수(3:7, v/v)용액제취양품중적피측물,재가입록화납,사용50 mg/mL N-병기을이알( PSA)+50 mg/mL 중성양화려( Alumina-N)적혼합분산고상췌취( dispersive solid phase extraction,DSPE)분말정화제취,과0.22μm 려막후이초고효액상색보-고분변천련질보검측。선택 Waters Acquity UPLC? BEH C8색보주(100 mm×2.1 mm,1.7μm),이갑순-5 mmol/L작산안수용액위류동상진행제도세탈。사용정、부리자동시소묘모식,기질외표법정량。연구표명,6충목표화합물적선성범위위:이초탁알,1.0~30.0μg/L;니잡파진,0.2~6.0μg/L;지극주리、타곡주리,2.0~60.0μg/L;막능균소、염매소,4.0~120.0μg/L。공백양품중첨가저、중、고3개수평적혼합표준용액,회수솔재67.7%~126.8%지간,상대표준편차( RSD )≤10.4%。6충항구충약물적정량한분별위:이초탁알,2.50μg/kg;니잡파진,0.50μg/kg;지극주리、타곡주리,5.00μg/kg;막능균소、염매소,20.00μg/kg。해방법조작간편,령민도고,차능구만족일상검측요구。
An ultra high liquid chromatography-Q Exactive orbitrap mass spectrometry multi-residue method has been developed for the determination of six anticoccidials residues (dinitlmide,nicarbazin,diclazuril,toltrazuril,monensin and salinomycin)in chicken tissue. Sample preparation was based on QuEChERS method,using 1%( v/v)trichloroacetic acid/acetonitrile aqueous solution(3:7,v/v)as the extraction solvent and salting-out with sodium chloride followed by clean-up with 50 mg/mL primary secondary amine( PSA)+50 mg/mL neu-tral alumina( Alumina-N ) dispersive solid phase extraction ( DSPE ). The separation of the compounds in liquid chromatography was carried out using a Waters Acquity UPLC ? BEH C8 column( 100 mm × 2. 1 mm,1. 7 μm ) with mobile phases consisting of methanol-5 mmol/L ammonium acetate aqueous solution in gradient elution. The Q Exactive orbitrap mass spectrometric detection was carried out with positive and negative electrospray ionization simul-taneously. The results showed the linear ranges of the six target compounds were as follows:dinitolmide,1. 0-30. 0 μg/L;nicarbazin,0. 2-6. 0 μg/L;diclazuril and toltrazuril,2. 0-60. 0μg/L;monensin and salinomycin,4. 0-120. 0 μg/L. The external standard method was used for quantification. The spiked recoveries at three levels for the six anticoccidials ranged from 67. 7% to 126. 8%. The relative standard deviations( RSDs)were ≤10. 4%. The limits of quanti-fication( LOQs)were as follows:dinitolmide,2. 50 μg/kg;nicarbazin,0. 50 μg/kg;diclazuril and toltrazuril,5. 00 μg/kg;monensin and salinomycin,20. 00 μg/kg. The developed method is easy of operation and of high sensitivity. It can meet the requirements of daily inspection.