高效液相色谱-串联质谱法测定奶粉中的壬基酚

Determination of nonylphenol in milk powder by high performance liquid chromatography-tandem mass spectrometry

研究利用高效液相色谱-串联质谱法（HPLC-MS／MS）快速准确测定婴幼儿配方奶粉中壬基酚。奶粉样品经水溶解后，乙腈提取所含的壬基酚，饱和氯化钠分离乙腈；以0．1％氨水溶液和乙腈作为流动相，以电喷雾离子源在负离子多反应监测模式进行上清液的测定。方法的检出限为0．76ng／mL，在1-400ng／mL范围内线性关系良好，相关系数为0．9997，方法回收率为84．3％-114．5％，RSD为4．78%-7．23％。方法快速、灵敏度高，适用于奶粉中壬基酚的测定。

Determination of nonylphenol in infant milk powder by high performance liquid chromatography-tandem mass spectrometry. Milk powder was dissolved in water, then nonylphenol was extracted with acetonitrile. Saturated sodium chloride was used to separate aceto- nitrile from water. The supernatant was separated with acetonitrile and 0.1% ammonia solution in water as eluents, and then detected with negative electrospray ionization under multiple reaction monitoring （MRM） mode. The results showed that the linear range was 1-400 rig/ mL （r=0.9997）, and the limit of detection was 0.76ng/mL. The mean recoveries of nonylphenol were 84.3%-114.5% with the relative stan- dard deviations of 4.78%-7.23%. The method is rapid, sensitive and suitable for the determination of nonylphenol in milk powder.