中国兽药杂志
中國獸藥雜誌
중국수약잡지
CHINESE JOURNAL OF VETERINARY DRUG
2015年
2期
27-30,31
,共5页
张强%张丹%刘业好%盛杰%陈文军%王国秀%刘开永
張彊%張丹%劉業好%盛傑%陳文軍%王國秀%劉開永
장강%장단%류업호%성걸%진문군%왕국수%류개영
磺胺间甲氧嘧啶%N4-乙酰化磺胺间甲氧嘧啶%高效液相色谱%二极管阵列检测器
磺胺間甲氧嘧啶%N4-乙酰化磺胺間甲氧嘧啶%高效液相色譜%二極管陣列檢測器
광알간갑양밀정%N4-을선화광알간갑양밀정%고효액상색보%이겁관진렬검측기
sulfamonomethoxine%N4- acetyl sulfamonomethoxine%high performance liquid chromatography%diode array detector
磺胺间甲氧嘧啶( SMM)于ICR小鼠哺乳期暴露后,测定其血清中SMM和N4-乙酰化磺胺间甲氧嘧啶(ACSMM)含量。小鼠哺乳期以0、10、50、200 mg/(kg·d)灌胃给药直至21 d,于第22天麻醉,摘眼球取血。血清样品经乙腈沉淀蛋白,超声辅助提取,采用反相 C18(250 mm ×4.6 mm,5μm)色谱柱,以乙腈:水(含0.2%冰乙酸)为流动相,流速为1 mL/min,柱温35℃,高效液相色谱耦合二极管阵列检测器对目标物检测,SMM和ACSMM检测波长分别为273 nm和267 nm,外标法峰面积定量。 SMM和ACSMM血清加标回收率为85.8%~110.2%,精密度( RSD%)均小于8.3%,在0.05~2.5μg/mL和5~30μg/mL(适用母鼠体内SMM)范围内与峰面积呈良好的线性关系,r2>0.990;最低检出限分别为0.023和0.042μg/mL。本法灵敏、快速、准确,可用于血清中SMM和ACSMM的测定。
磺胺間甲氧嘧啶( SMM)于ICR小鼠哺乳期暴露後,測定其血清中SMM和N4-乙酰化磺胺間甲氧嘧啶(ACSMM)含量。小鼠哺乳期以0、10、50、200 mg/(kg·d)灌胃給藥直至21 d,于第22天痳醉,摘眼毬取血。血清樣品經乙腈沉澱蛋白,超聲輔助提取,採用反相 C18(250 mm ×4.6 mm,5μm)色譜柱,以乙腈:水(含0.2%冰乙痠)為流動相,流速為1 mL/min,柱溫35℃,高效液相色譜耦閤二極管陣列檢測器對目標物檢測,SMM和ACSMM檢測波長分彆為273 nm和267 nm,外標法峰麵積定量。 SMM和ACSMM血清加標迴收率為85.8%~110.2%,精密度( RSD%)均小于8.3%,在0.05~2.5μg/mL和5~30μg/mL(適用母鼠體內SMM)範圍內與峰麵積呈良好的線性關繫,r2>0.990;最低檢齣限分彆為0.023和0.042μg/mL。本法靈敏、快速、準確,可用于血清中SMM和ACSMM的測定。
광알간갑양밀정( SMM)우ICR소서포유기폭로후,측정기혈청중SMM화N4-을선화광알간갑양밀정(ACSMM)함량。소서포유기이0、10、50、200 mg/(kg·d)관위급약직지21 d,우제22천마취,적안구취혈。혈청양품경을정침정단백,초성보조제취,채용반상 C18(250 mm ×4.6 mm,5μm)색보주,이을정:수(함0.2%빙을산)위류동상,류속위1 mL/min,주온35℃,고효액상색보우합이겁관진렬검측기대목표물검측,SMM화ACSMM검측파장분별위273 nm화267 nm,외표법봉면적정량。 SMM화ACSMM혈청가표회수솔위85.8%~110.2%,정밀도( RSD%)균소우8.3%,재0.05~2.5μg/mL화5~30μg/mL(괄용모서체내SMM)범위내여봉면적정량호적선성관계,r2>0.990;최저검출한분별위0.023화0.042μg/mL。본법령민、쾌속、준학,가용우혈청중SMM화ACSMM적측정。
Determination of sulfamonomethoxine ( SMM ) and N4-acetyl metabolite ( ACSMM ) in ICR mice exposed to SMM during lactation. The lactational mice were orally administered with SMM ( 0, 10, 50, 200 mg/( kg·d) for 21 d, the mice were anesthetized and then taken blood by removalling eyeball. Following serum protein precipitation with acetonitrile, the ultrasonic- assisted extraction of the targets, separation of them were carried out on a reversed-phase C18 (250 mm×4.6 mm, 5μm) column, the mobile phase was involved in acetonitrile and 0.2% acetic acid in water, the flow rate was 1 mL/min and the column temperature was 35 ℃, the high performance liquid chromatography was coupled with a diode array detector, detection wavelength of SMM and ACSMM were 273 and 267 nm respectively, and quantified with external standard method. The recoveries of SMM and ACSMM spiked in serum were 85.8% ~110.2%, RSDs less than 8.3% were obtained, the linear range was 0.05~2.5 μg/mL, but 5~30 μg/mL suitable for SMM in the dams, and showed a good linear relationship ( r2>0. 990 ) . The limit of quantitation ( LOQ ) was 0. 023 and 0. 042 μg/mL respectively. This method was sensitive, rapid, accurate, can be used for the determination of SMM and ACSMM in serum.