色谱
色譜
색보
CHINESE JOURNAL OF CHROMATOGRAPHY
2014年
5期
519-523
,共5页
李帅鹏%郭春娜%孟蕾%黄显会
李帥鵬%郭春娜%孟蕾%黃顯會
리수붕%곽춘나%맹뢰%황현회
高效液相色谱%串联质谱%头孢洛宁%牛奶%残留
高效液相色譜%串聯質譜%頭孢洛寧%牛奶%殘留
고효액상색보%천련질보%두포락저%우내%잔류
high performance liquid chromatography ( HPLC )%tandem mass spectrometry ( MS/MS)%cefalonium%milk%residue
建立了牛奶中头孢洛宁残留检测的高效液相色谱-串联质谱方法。1g 牛奶经乙腈沉淀蛋白质后,上清液于37℃水浴下氮气吹干,用1 mL甲醇-0.1%甲酸水溶液(3:7,v/v)复溶,正己烷除脂净化后检测。流动相为乙腈和0.1%甲酸水溶液,梯度洗脱,经 C18色谱柱分离,采用多反应监测正离子模式对头孢洛宁进行定性定量分析。采用基质匹配法对牛奶中头孢洛宁的含量进行标准校正,在2~200μg/L范围内,头孢洛宁质量浓度与其对应峰面积的线性关系良好,相关系数﹥0.999。牛奶中加标样品的检出限(按S/N≥3计)为0.5μg/kg,定量限( S/N≥10计)为2μg/kg。在定量限、1/2最高残留限量、最高残留限量、2倍最高残留限量添加水平下,牛奶中头孢洛宁的平均回收率为78.5%~86.2%,日内相对标准偏差为1.5%~6.2%,日间相对标准偏差为2.9%~5.6%。该方法可用于牛奶中头孢洛宁的残留检测。
建立瞭牛奶中頭孢洛寧殘留檢測的高效液相色譜-串聯質譜方法。1g 牛奶經乙腈沉澱蛋白質後,上清液于37℃水浴下氮氣吹榦,用1 mL甲醇-0.1%甲痠水溶液(3:7,v/v)複溶,正己烷除脂淨化後檢測。流動相為乙腈和0.1%甲痠水溶液,梯度洗脫,經 C18色譜柱分離,採用多反應鑑測正離子模式對頭孢洛寧進行定性定量分析。採用基質匹配法對牛奶中頭孢洛寧的含量進行標準校正,在2~200μg/L範圍內,頭孢洛寧質量濃度與其對應峰麵積的線性關繫良好,相關繫數﹥0.999。牛奶中加標樣品的檢齣限(按S/N≥3計)為0.5μg/kg,定量限( S/N≥10計)為2μg/kg。在定量限、1/2最高殘留限量、最高殘留限量、2倍最高殘留限量添加水平下,牛奶中頭孢洛寧的平均迴收率為78.5%~86.2%,日內相對標準偏差為1.5%~6.2%,日間相對標準偏差為2.9%~5.6%。該方法可用于牛奶中頭孢洛寧的殘留檢測。
건립료우내중두포락저잔류검측적고효액상색보-천련질보방법。1g 우내경을정침정단백질후,상청액우37℃수욕하담기취간,용1 mL갑순-0.1%갑산수용액(3:7,v/v)복용,정기완제지정화후검측。류동상위을정화0.1%갑산수용액,제도세탈,경 C18색보주분리,채용다반응감측정리자모식대두포락저진행정성정량분석。채용기질필배법대우내중두포락저적함량진행표준교정,재2~200μg/L범위내,두포락저질량농도여기대응봉면적적선성관계량호,상관계수﹥0.999。우내중가표양품적검출한(안S/N≥3계)위0.5μg/kg,정량한( S/N≥10계)위2μg/kg。재정량한、1/2최고잔류한량、최고잔류한량、2배최고잔류한량첨가수평하,우내중두포락저적평균회수솔위78.5%~86.2%,일내상대표준편차위1.5%~6.2%,일간상대표준편차위2.9%~5.6%。해방법가용우우내중두포락저적잔류검측。
An analytical method was developed for the determination of cefalonium in milk by high performance liquid chromatography-tandem mass spectrometry( HPLC-MS/MS). A total of 1g milk was deproteinized by acetonitrile. The supernatant was transferred into a test tube to be blown dry with N2 at 37 ℃.Then the residue was dissolved with methanol-0.1% formic acid in water(3:7,v/v). The sample was determined by HPLC-MS/MS after the purification.The chromatographic separation was achieved on a C18 column using 0.1% formic acid in water and acetonitrile as mobile phases with gradient elution. Qualitative and quantitative analyses were achieved by HPLC-MS/MS under positive ionization and multiple reaction monitoring( MRM ) mode.Matrix-matched calibration curve was used for the quantification. Good correlation coef-ficients were obtained( r﹥0. 999)in the mass concentration range of 2-200 μg/L. The limit of detection( LOD,S/N≥3)was 0. 5 μg/kg in milk,and the limit of quantification( LOQ,S/N≥10)was 2 μg/kg. The mean recoveries at the four levels of LOQ,1/2MRL( maximum residue level),MRL,2MRL were between 78. 5% and 86. 2%,with the intra-day relative standard devi-ations( RSDs)of 1. 5% to 6. 2% and inter-day RSDs of 2. 9% to 5. 6%. In conclusion,the estab-lished method can be applied for the determination of cefalonium residue in milk.