现代畜牧兽医
現代畜牧獸醫
현대축목수의
LIAONING JOURNAL OF ANIMAL HUSBANDRY AND VETERINARY MEDICINE
2013年
10期
38-42
,共5页
气相色谱- 质谱法%生鲜乳%己烯雌酚%雌二醇%炔雌醇
氣相色譜- 質譜法%生鮮乳%己烯雌酚%雌二醇%炔雌醇
기상색보- 질보법%생선유%기희자분%자이순%결자순
GC-MS%Milk%Diethylstilbestrol%Estradiol%Ethinylestradiol
本研究建立了测定生鲜乳中己烯雌酚(diethylstilbestrol)、雌二醇(estradiol)、炔雌醇(ethi-nylestradiol)、戊酸雌二醇(estradiol valerate)残留量的GC- MS法,为控制食源性动物食品的质量安全提供依据。本试验的样品经乙腈和乙酸乙酯提取,HLB固相萃取小柱净化,70℃衍生后在EI源SIM模式下进样分析。试验结果显示,己烯雌酚、雌二醇、炔雌醇含量在2.0~100.0μg/kg内、戊酸雌二醇含量在4.0~200.0μg/kg内线性关系良好,己烯雌酚、雌二醇、炔雌醇、戊酸雌二醇相关系数分别为0.9991、0.9987、0.9978、0.9983,平均回收率(n=6)为74.2%~85.8%(RSD为1.9%~9.2%)。该方法能够为测定生鲜乳中这4种雌激素类药物残留量提供可靠依据。
本研究建立瞭測定生鮮乳中己烯雌酚(diethylstilbestrol)、雌二醇(estradiol)、炔雌醇(ethi-nylestradiol)、戊痠雌二醇(estradiol valerate)殘留量的GC- MS法,為控製食源性動物食品的質量安全提供依據。本試驗的樣品經乙腈和乙痠乙酯提取,HLB固相萃取小柱淨化,70℃衍生後在EI源SIM模式下進樣分析。試驗結果顯示,己烯雌酚、雌二醇、炔雌醇含量在2.0~100.0μg/kg內、戊痠雌二醇含量在4.0~200.0μg/kg內線性關繫良好,己烯雌酚、雌二醇、炔雌醇、戊痠雌二醇相關繫數分彆為0.9991、0.9987、0.9978、0.9983,平均迴收率(n=6)為74.2%~85.8%(RSD為1.9%~9.2%)。該方法能夠為測定生鮮乳中這4種雌激素類藥物殘留量提供可靠依據。
본연구건립료측정생선유중기희자분(diethylstilbestrol)、자이순(estradiol)、결자순(ethi-nylestradiol)、무산자이순(estradiol valerate)잔류량적GC- MS법,위공제식원성동물식품적질량안전제공의거。본시험적양품경을정화을산을지제취,HLB고상췌취소주정화,70℃연생후재EI원SIM모식하진양분석。시험결과현시,기희자분、자이순、결자순함량재2.0~100.0μg/kg내、무산자이순함량재4.0~200.0μg/kg내선성관계량호,기희자분、자이순、결자순、무산자이순상관계수분별위0.9991、0.9987、0.9978、0.9983,평균회수솔(n=6)위74.2%~85.8%(RSD위1.9%~9.2%)。해방법능구위측정생선유중저4충자격소류약물잔류량제공가고의거。
This research to develop and validate a rapid sensitive and specific meth-od for quantitative analytes of estrogens residues(DES, Diethylstilbestrol: E2, Es-tradiol: EE2, Ethynylestradiol: EV, Estradiol Valerate)in milk by gas chromatograph-ic-tandem mass spectrometry and be applied to estrogens residues in milk studies. The 4 kinds of components were extracted from homogenized samples with ethyl acetate fol-lowed by solid-phase extraction with HLB column and trimethylsilylation at 70 ℃ for 40 minutes, then the GC-MS method in selected ion monitoring mode(SIM)was used to an-alyze them. A good linearity was achieved with the coefficient r2 > 0.997 8(n =2). The average recovery of estrogens was more than 74.2% with RSD lower than 9.2%(n = 9). The method is sensitive, accurate, rapid, and suitable for the analysis estrogens resi-dues in milk.