高效液相色谱-荧光检测法测定鱼类和贝类中的4-壬基酚、壬基酚单乙氧基化物、壬基酚二乙氧基化物及其他烷基酚
Determination of 4-nonylphenol, nonylphenol monoethoxylate, nonylphenol diethoxylate and other alkylphenols in fish and shellfish by high-performance liquid chromatography with fluorescence detection.
作者信息
Tsuda T, Suga K, Kaneda E, Ohsuga M
机构信息
Shiga Prefectural Kusatsu Public Health Center, Japan.
出版信息
J Chromatogr B Biomed Sci Appl. 2000 Sep 15;746(2):305-9. doi: 10.1016/s0378-4347(00)00322-4.
A simple and highly sensitive method is described for the HPLC determination of 4-nonylphenol (NP), 4-nonylphenol mono- (NP1EO) and diethoxylates (NP2EO) in fish and shellfish together with bisphenol A (BPA), 4-tert.-butylphenol (BP) and 4-tert.-octylphenol (OP). The NP, NP1EO, NP2EO and other alkylphenols in the samples are extracted with acetonitrile and the lipid in the sample extract is eliminated by partitioning between hexane and acetonitrile. After Florisil PR clean-up the sample extract is analyzed by HPLC with a fluorescence detection. Recoveries in Japanese smelt, carp and corbicura are 81.8-84.3% for NP, 83.5-84.3% for NP1EO, 90.5-96.2% for NP2EO, 70.7-72.9% for BPA, 71.0-73.4% for BP and 77.1-83.2% for OP spiked at 0.5 microg each chemical per 5 g of the fish and shellfish samples. The detection limits are 2 ng/g for NP, NP1EO and NP2EO, and 1ng/g for BPA, BP and OP.
本文描述了一种简单且高灵敏度的方法，用于通过高效液相色谱法（HPLC）测定鱼类和贝类中的4-壬基酚（NP）、4-壬基酚单乙氧基化物（NP1EO）和二乙氧基化物（NP2EO），同时测定双酚A（BPA）、4-叔丁基酚（BP）和4-叔辛基酚（OP）。样品中的NP、NP1EO、NP2EO和其他烷基酚用乙腈萃取，样品萃取液中的脂质通过正己烷和乙腈之间的分配去除。经弗罗里硅土PR净化后，样品萃取液用带荧光检测的HPLC进行分析。在日本胡瓜鱼、鲤鱼和蚬中，每种化学物质以每5克鱼类和贝类样品0.5微克的量加标时，NP的回收率为81.8 - 84.3%，NP1EO为83.5 - 84.3%，NP2EO为90.5 - 96.2%，BPA为70.7 - 72.9%，BP为71.0 - 73.4%，OP为77.1 - 83.2%。NP、NP1EO和NP2EO的检测限为2纳克/克，BPA、BP和OP的检测限为1纳克/克。
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