中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2012年
11期
27-30
,共4页
高玲%张丹%高峰%郭栋%杨瑞章%于伯华
高玲%張丹%高峰%郭棟%楊瑞章%于伯華
고령%장단%고봉%곽동%양서장%우백화
水产品%氨基糖苷%残留检测%高效液相色谱-串联质谱
水產品%氨基糖苷%殘留檢測%高效液相色譜-串聯質譜
수산품%안기당감%잔류검측%고효액상색보-천련질보
aquatic products%aminoglycoside%residue detection%LC - MS/MS
建立了高效液相色谱一串联质谱方法测定水产品中链霉素、双氢链霉素、新霉素、庆大霉素和卡那霉素5种氨基糖苷类抗生素的检测方法。样品中的氨基糖苷类抗生素用磷酸缓冲溶液提取液提取后,经固相萃取进行净化,改进了前处理方法,并对液相和质谱的条件进行了优化。通过实际样品的添加回收试验,方法的定量下限(S/N=10)为10.0μg,/kg。三个添加水平分别为10.0、20.0和50.0μg/kg时,龙虾、鲴鱼的加标回收率均在60%一110%,日内相对标准偏差不超过15.0%。结果表明,该方法简单、灵敏、特异性强,适用于水产品中氨基糖苷类药物残留的检测和确证。
建立瞭高效液相色譜一串聯質譜方法測定水產品中鏈黴素、雙氫鏈黴素、新黴素、慶大黴素和卡那黴素5種氨基糖苷類抗生素的檢測方法。樣品中的氨基糖苷類抗生素用燐痠緩遲溶液提取液提取後,經固相萃取進行淨化,改進瞭前處理方法,併對液相和質譜的條件進行瞭優化。通過實際樣品的添加迴收試驗,方法的定量下限(S/N=10)為10.0μg,/kg。三箇添加水平分彆為10.0、20.0和50.0μg/kg時,龍蝦、鲴魚的加標迴收率均在60%一110%,日內相對標準偏差不超過15.0%。結果錶明,該方法簡單、靈敏、特異性彊,適用于水產品中氨基糖苷類藥物殘留的檢測和確證。
건립료고효액상색보일천련질보방법측정수산품중련매소、쌍경련매소、신매소、경대매소화잡나매소5충안기당감류항생소적검측방법。양품중적안기당감류항생소용린산완충용액제취액제취후,경고상췌취진행정화,개진료전처리방법,병대액상화질보적조건진행료우화。통과실제양품적첨가회수시험,방법적정량하한(S/N=10)위10.0μg,/kg。삼개첨가수평분별위10.0、20.0화50.0μg/kg시,룡하、고어적가표회수솔균재60%일110%,일내상대표준편차불초과15.0%。결과표명,해방법간단、령민、특이성강,괄용우수산품중안기당감류약물잔류적검측화학증。
A high performance liquid chromatography- tandem mass spectrometric (HPLC -MS/MS) method was developed for the determination of five aminoglycosides drugs such as streptomycin, dihydrostreptomycin, kanamycin, gentamicin and neomycinb in aquatic products. The aminoglycosides drugs interested were extracted from the samples with phosphate buffer solution and separated by a cation exchange chromatographic column. An improved pre- treatment method was used in this study and the eluent solution types and chromatographic parameters were optimized. In the detection of spiked samples, the detection limite of this method was 10.0 μg/kg (S/N = 10) for the five durgs spiked in fish and crayfish respectively, which can match the requirement of the supervision. The recoveries of the five durgs from fish and crayfish samples spiked with three concentration levels of 10.0, 20.0 and 50.0 μg./kg ranged from 60% to 110% with RSD less than 15.0%. The established method was accurate, sensitive and simple, and was suitable for the quantification of aminoglycosides antibiotics residue in aquatic products.