农业环境科学学报
農業環境科學學報
농업배경과학학보
Journal of Agro-Environment Science
2014年
5期
1050-1056
,共7页
刘博%薛南冬%杨兵%龚道新%李发生%张石磊%周玲莉%孟磊%陈宣宇%燕云仲
劉博%薛南鼕%楊兵%龔道新%李髮生%張石磊%週玲莉%孟磊%陳宣宇%燕雲仲
류박%설남동%양병%공도신%리발생%장석뢰%주령리%맹뢰%진선우%연운중
氟喹诺酮类抗生素%固相萃取-高效液相色谱荧光检测法(SPE-HPLC/FLD)%禽畜粪便%分析方法
氟喹諾酮類抗生素%固相萃取-高效液相色譜熒光檢測法(SPE-HPLC/FLD)%禽畜糞便%分析方法
불규낙동류항생소%고상췌취-고효액상색보형광검측법(SPE-HPLC/FLD)%금축분편%분석방법
fluoroquinolones(FQs)%solid-phase extraction-high performance liquid chromatography with fluorescence detection%livestock and poultry excrement%analytical method
通过对样品预处理过程优化、提取剂与洗脱剂的筛选和检测色谱条件优化，建立了基于固相萃取-高效液相色谱荧光检测法分析鸡粪中6种氟喹诺酮类（云匝泽）的检测方法。该方法选用Mcllvaine-Na2EDTA缓冲液颐乙腈（1：1，V/V）（pH=2）作为提取剂，超声提取时间15 min，经HLB固相柱净化，选用甲醇为洗脱剂，浓缩后用HPLC/FLD检测，采用乙腈/0.7%磷酸作为流动相。FQs在0.01~1.0 mg·kg-1浓度范围内呈现良好线性关系，R2为0.9969~0.9999。加标（浓度水平0.01、0.5、1.0 mg·kg-1干重）回收率达76.7%~106.7%，相对标准偏差0.7%~14.4%（n=4）。方法检出限为0.002~0.022 mg·kg-1，方法定量限为0.0068~0.074 mg·kg-1。应用该方法对北京地区5个养鸡场内鸡粪样品中6种FQs进行分析，检出浓度为ND~1.13 mg·kg-1。
通過對樣品預處理過程優化、提取劑與洗脫劑的篩選和檢測色譜條件優化，建立瞭基于固相萃取-高效液相色譜熒光檢測法分析鷄糞中6種氟喹諾酮類（雲匝澤）的檢測方法。該方法選用Mcllvaine-Na2EDTA緩遲液頤乙腈（1：1，V/V）（pH=2）作為提取劑，超聲提取時間15 min，經HLB固相柱淨化，選用甲醇為洗脫劑，濃縮後用HPLC/FLD檢測，採用乙腈/0.7%燐痠作為流動相。FQs在0.01~1.0 mg·kg-1濃度範圍內呈現良好線性關繫，R2為0.9969~0.9999。加標（濃度水平0.01、0.5、1.0 mg·kg-1榦重）迴收率達76.7%~106.7%，相對標準偏差0.7%~14.4%（n=4）。方法檢齣限為0.002~0.022 mg·kg-1，方法定量限為0.0068~0.074 mg·kg-1。應用該方法對北京地區5箇養鷄場內鷄糞樣品中6種FQs進行分析，檢齣濃度為ND~1.13 mg·kg-1。
통과대양품예처리과정우화、제취제여세탈제적사선화검측색보조건우화，건립료기우고상췌취-고효액상색보형광검측법분석계분중6충불규낙동류（운잡택）적검측방법。해방법선용Mcllvaine-Na2EDTA완충액이을정（1：1，V/V）（pH=2）작위제취제，초성제취시간15 min，경HLB고상주정화，선용갑순위세탈제，농축후용HPLC/FLD검측，채용을정/0.7%린산작위류동상。FQs재0.01~1.0 mg·kg-1농도범위내정현량호선성관계，R2위0.9969~0.9999。가표（농도수평0.01、0.5、1.0 mg·kg-1간중）회수솔체76.7%~106.7%，상대표준편차0.7%~14.4%（n=4）。방법검출한위0.002~0.022 mg·kg-1，방법정량한위0.0068~0.074 mg·kg-1。응용해방법대북경지구5개양계장내계분양품중6충FQs진행분석，검출농도위ND~1.13 mg·kg-1。
An analytical method for simultaneous determination of six fluoroquinolones(FQs)in chicken manures based on solid-phase ex-traction and high performance liquid chromatography with a fluorescence detection(HPLC/FLD)was developed in the current study. Sam-ples were ultrasonically extracted in Mcllvaine-Na2EDTA buffer/acetonitrile(1:1)(pH=2)for 15 min. The extract was cleaned by a HLB solid-phase extraction column, and then eluted with methanol solvent. The fluoroquinolones in the extract were determined by HPLC/FLD with acetonitrile/0.7%phosphate as mobile phase. In a concentration range of 0.01~1.0 mg·kg-1, R2 of calibration was greater than 0.99. The average percent recoveries ranged from 76.7%to 106.7%for six compounds in chicken manure samples at three different spiked levels(0.1, 0.5 mg·kg-1 and 1.0 mg·kg-1). The detection limits(LOD)were from 0.002 mg·kg-1 to 0.022 mg·kg-1, and limit of quantification(LOQ) from 0.006 8 mg·kg-1 to 0.074 mg·kg-1. This method was used to analyze six FQs in chicken manures collected from 5 chicken farms in Beijing. All six FQs were detected in most samples, with concentrations ranging from LOD to 1.13 mg·kg-1.
