色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
7期
702-706
,共5页
孙婷%王鹭骁%曾三妹%吴敏%严丽娟%张峰%黄志强
孫婷%王鷺驍%曾三妹%吳敏%嚴麗娟%張峰%黃誌彊
손정%왕로효%증삼매%오민%엄려연%장봉%황지강
固相萃取%超高效液相色谱-电喷雾串联质谱%精神药物%猪肉
固相萃取%超高效液相色譜-電噴霧串聯質譜%精神藥物%豬肉
고상췌취%초고효액상색보-전분무천련질보%정신약물%저육
solid phase extraction( SPE )%ultra performance liquid chromatography-electro-spary ionization tandem mass spectrometry( UPLC-ESI-MS/MS)%psychoactive drugs%pork
建立了固相萃取和超高效液相色谱-电喷雾串联质谱( UPLC-ESI-MS/MS)同时测定猪肉中20种精神药物残留的方法。样品采用碱性乙腈作为提取试剂,提取液经 Oasis MCX固相萃取柱净化后,以含0.1%( v/v)甲酸的水溶液和乙腈作为流动相梯度洗脱,用 C18色谱柱分离,正离子模式扫描,多反应监测模式检测。20种化合物在5~100μg/L质量浓度范围内均呈良好的线性关系,线性相关系数均大于0.99,以 S/N≥10计算方法的定量限为5μg/kg。在空白猪肉中添加5、10和50μg/kg 水平的20种药物,其平均回收率为66.8%~97.2%,相对标准偏差( RSD)为4.2%~12.4%。本方法快速、准确、可靠,适用于猪肉中精神药物多残留的同时测定。
建立瞭固相萃取和超高效液相色譜-電噴霧串聯質譜( UPLC-ESI-MS/MS)同時測定豬肉中20種精神藥物殘留的方法。樣品採用堿性乙腈作為提取試劑,提取液經 Oasis MCX固相萃取柱淨化後,以含0.1%( v/v)甲痠的水溶液和乙腈作為流動相梯度洗脫,用 C18色譜柱分離,正離子模式掃描,多反應鑑測模式檢測。20種化閤物在5~100μg/L質量濃度範圍內均呈良好的線性關繫,線性相關繫數均大于0.99,以 S/N≥10計算方法的定量限為5μg/kg。在空白豬肉中添加5、10和50μg/kg 水平的20種藥物,其平均迴收率為66.8%~97.2%,相對標準偏差( RSD)為4.2%~12.4%。本方法快速、準確、可靠,適用于豬肉中精神藥物多殘留的同時測定。
건립료고상췌취화초고효액상색보-전분무천련질보( UPLC-ESI-MS/MS)동시측정저육중20충정신약물잔류적방법。양품채용감성을정작위제취시제,제취액경 Oasis MCX고상췌취주정화후,이함0.1%( v/v)갑산적수용액화을정작위류동상제도세탈,용 C18색보주분리,정리자모식소묘,다반응감측모식검측。20충화합물재5~100μg/L질량농도범위내균정량호적선성관계,선성상관계수균대우0.99,이 S/N≥10계산방법적정량한위5μg/kg。재공백저육중첨가5、10화50μg/kg 수평적20충약물,기평균회수솔위66.8%~97.2%,상대표준편차( RSD)위4.2%~12.4%。본방법쾌속、준학、가고,괄용우저육중정신약물다잔류적동시측정。
A method for the simultaneous determination of 20 psychoactive drugs in pork by solid phase extraction coupled with ultra performance liquid chromatography with electrospray ionization tandem mass spectrometry( UPLC-ESI-MS/MS)was established. The samples were extracted with alkalified acetonitrile,and then cleaned up using solid phase extraction with an Oasis MCX column. The UPLC separation was performed on a C18 column( 50 mm × 2. 1 mm, 1. 7 μm)using a gradient elution with the mobile phases of 0. 1%( v/v)formic acid in water and acetonitrile. The ESI-MS/MS detection was achieved in positive mode under multiple reac-tion monitoring( MRM)mode. The calibration curves showed good linearity in the range of 5-100 μg/L with the correlation coefficients more than 0. 99 for the 20 psychoactive drugs. The limits of quantification( LOQ,S/N≥10)for the 20 psychoactive drugs were 5 μg/kg. The aver-age recoveries of the 20 psychoactive drugs spiked in blank pork at three levels of 5,10 and 50μg/kg were 66. 8%-97. 2% with the relative standard deviations from 4. 2% to 12. 4%. The meth-od is suitable for the simultaneous determination of the 20 psychoactive drugs in pork with the characteristics of easy operation,high accuracy and precision.