中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2014年
9期
40-44,45
,共6页
张金玲%孙礼瑞%谢恺舟%张小杰%李凯
張金玲%孫禮瑞%謝愷舟%張小傑%李凱
장금령%손례서%사개주%장소걸%리개
阿莫西林%荧光法%鸡组织%高效液相色谱
阿莫西林%熒光法%鷄組織%高效液相色譜
아막서림%형광법%계조직%고효액상색보
amoxicillin ( AMO)%fluorescence detection%chicken tissue%HPLC
建立了高效液相色谱荧光法检测鸡组织中阿莫西林( AMO )的残留量。鸡组织样品经磷酸二氢钠溶液提取,乙腈去蛋白,正己烷去脂肪,饱和二氯甲烷萃取,上清液经水杨醛在酸性条件下沸水浴衍生化。以0.01 mol/L 的磷酸二氢钾溶液和乙腈溶液为流动相,梯度洗脱,流速为1 mL/min,高效液相色谱荧光检测,激发波长为358 nm,发射波长为440 nm。阿莫西林在25~1000μg/kg质量浓度范围内,线性关系良好。当阿莫西林添加水平为13~125μg/kg时,鸡组织中AMO的平均回收率在72.82%~88.82%,相对标准偏差在6.21%~9.63%;检测限、定量限分别为5μg/kg(S/N≥3)、13μg/kg(S/N≥10)。该方法操作简便,可适用于鸡组织中阿莫西林的提取和检测,且准确度和精密度均符合残留分析的要求。
建立瞭高效液相色譜熒光法檢測鷄組織中阿莫西林( AMO )的殘留量。鷄組織樣品經燐痠二氫鈉溶液提取,乙腈去蛋白,正己烷去脂肪,飽和二氯甲烷萃取,上清液經水楊醛在痠性條件下沸水浴衍生化。以0.01 mol/L 的燐痠二氫鉀溶液和乙腈溶液為流動相,梯度洗脫,流速為1 mL/min,高效液相色譜熒光檢測,激髮波長為358 nm,髮射波長為440 nm。阿莫西林在25~1000μg/kg質量濃度範圍內,線性關繫良好。噹阿莫西林添加水平為13~125μg/kg時,鷄組織中AMO的平均迴收率在72.82%~88.82%,相對標準偏差在6.21%~9.63%;檢測限、定量限分彆為5μg/kg(S/N≥3)、13μg/kg(S/N≥10)。該方法操作簡便,可適用于鷄組織中阿莫西林的提取和檢測,且準確度和精密度均符閤殘留分析的要求。
건립료고효액상색보형광법검측계조직중아막서림( AMO )적잔류량。계조직양품경린산이경납용액제취,을정거단백,정기완거지방,포화이록갑완췌취,상청액경수양철재산성조건하비수욕연생화。이0.01 mol/L 적린산이경갑용액화을정용액위류동상,제도세탈,류속위1 mL/min,고효액상색보형광검측,격발파장위358 nm,발사파장위440 nm。아막서림재25~1000μg/kg질량농도범위내,선성관계량호。당아막서림첨가수평위13~125μg/kg시,계조직중AMO적평균회수솔재72.82%~88.82%,상대표준편차재6.21%~9.63%;검측한、정량한분별위5μg/kg(S/N≥3)、13μg/kg(S/N≥10)。해방법조작간편,가괄용우계조직중아막서림적제취화검측,차준학도화정밀도균부합잔류분석적요구。
To develop a high performance liquid chromatography with fluorescence detection ( HPLC-FLD ) method for determination of residues of amoxicillin ( AMO) in chicken tissues, AMO were extracted from chicken tissues with sodium dihydrogen phosphate solution. After being deproteinizated with acetonitrile and degreased in n-hexane saturated, the analyte was extracted by saturated dichloromethane. The supernatant was reacted with salicylaldehyde under acidic and boiling conditions. The mobile phase were 0. 01 mol/L potassium dihydrogen phosphate and acetonitrile, the flow rate was 1 mL/min. Fluorescence detection was carried out at excitation and emission wavelengths of 358 nm and 440 nm. The calibration curves were linear in the range from 25 to 1000 μg/kg. At spiked level of 13~125 μg/kg for AMO, the average recoveries was 72. 82%~88. 82% with coefficients of variation between 6.21% and 9.63%. Limit of detection ( LOD) and limit of quantitation ( LOQ) were 5 μg/kg and 13 μg/kg, respectively. This HPLC-FLD method is simple, rapid, sensitive and reliable for the determination of residues of amoxicillin in chicken tissues.