离子色谱法测定奶制品及蜂王浆中的乙酰胆碱

Determination of Acetylcholine in Dairy Product and Royal Jelly by Ion Chromatography

建立了奶制品及蜂王浆中乙酰胆碱的离子交换／电导检测离子色谱分析方法。样品经去离子水超声提取，离子交换／电导检测离子色谱法测定，外标法定量。采用IonPac CS17（250mm×4．0mmi．d．）分析柱，流动相为甲基磺酸，梯度洗脱，流速1．0mL／min，柱温30℃，检测池温度35℃。实验结果表明，氯化乙酰胆碱在0．02～2．0mg／L范围内线性关系良好（r=0．9999），牛奶、酸奶、蜂王浆中乙酰胆碱的检出限为0．3mg／kg，奶粉为1mg／kg，不同基质中3个加标水平下的回收率为90％～98％，相对标准偏差为3．0％～6．2％。

A ionexchange chromatographic method with conductivity detection was developed for the determination of acetylcholine （Ach） residue in dairy products and royal jelly. The sample was extracted with ultra-pure water by ultrasonic, and then determined by ion chromatography. The quantification was performed by the external standard, using IonPac CS17（250 mm ×4.0 mm i. d. ） column as analytical column, and methylsulfonic acid （MSA）as mobile phase at a flow rate of 1.0 mL/min. The column temperature was set at 30 ℃, and the detection cell temperature was set at 35 ℃. The calibration curve was linear between the peak area and the Ach concentration in the range of 0.02 - 2.0 mg/L with a correlation coefficient of 0. 999 9. The limit of detection of Ach was 0.3 mg/kg in milk, yogurt and royal jelly matrices, and 1.0 mg/kg in milk powder matrix. The average recoveries of Ach from spiked daily products and royal jelly sample ranged from 90% to 98% with RSDs of 3.0% -6.2%.