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目的建立不同基质食品中双酚 A(BPA)、壬基酚(NP)和辛基酚(OP)等类雌激素的高压液相色谱法(HPLC),检测市售罐装食品中类雌激素。方法固体样品经甲醇超声提取、二氯甲烷萃取、浓缩。液体样品的分析采用 NH_2柱浓缩、富集和净化。HPLC 采用 Waters XTerra~(TM) MS C_(18)液相色谱柱分离,甲醇-水作为流动相梯度洗脱。采用荧光检测,激发波长:225 nm;发射波长:310 nm。结果建立的方法具有良好的线性关系,蔬菜类罐装食品和方便面中 BPA、NP 和 OP 的检出限分别为0.5、0.1和0.1μg/kg,鱼、肉类罐装食品 BPA、NP 和 OP 的检出限分别为1、0.5和0.5μg/kg。BPA、NP 和 OP 加标回收率分别为74.9%~95.1%、76.3%~103.6%和72.1%~109.2%;相对标准偏差(RSD)分别为4.98%~11.2%、2.35%~8.88%和5.61%~12.3%。结论该方法测定罐装食品及方便面中类雌激素(BPA、OP 和 NP),具有较高的灵敏度和选择性,结果准确可靠、重现性好。
OBJECTIVE To establish high pressure liquid chromatography (HPLC) of estrogen such as BPA, NP and OP in different matrices, . Methods Solid samples were extracted by methanol, extracted with dichloromethane and concentrated. Analysis of liquid samples using NH_2 column enrichment, enrichment and purification. The HPLC was separated on a Waters XTerra ~ (TM) MS C 18 (18) column using methanol-water as a mobile phase gradient. Fluorescence detection, excitation wavelength: 225 nm; emission wavelength: 310 nm. Results The established method has a good linear relationship. The detection limits of BPA, NP and OP in vegetable canned food and instant noodles are 0.5, 0.1 and 0.1 μg / kg, respectively. The fish and meat canned foods BPA, NP and OP The detection limits were 1, 0.5 and 0.5 μg / kg, respectively. The recoveries of BPA, NP and OP were 74.9% ~ 95.1%, 76.3% ~ 103.6% and 72.1% ~ 109.2%, respectively. The relative standard deviations (RSDs) were 4.98% ~ 11.2%, 2.35% ~ 8.88% and 5.61% % ~ 12.3%. Conclusion The method of determination of estrogen (BPA, OP and NP) in canned foods and instant noodles has high sensitivity and selectivity and the results are accurate and reliable with good reproducibility.