Yin Hua
Changshu Provincial Center for Disease Control and Prevention, Changshu 215500, China.
Wei Sheng Yan Jiu. 2017 Nov;46(6):971-980.
To establish a high performance liquid chromatographytandem mass spectrometry( HPLC-MS/MS) method for simultaneous determination of caffeine, benzoic acid, sorbic acid, acesulfame potassium, saccharin sodium and sodium cyclamate in drink.
The sample was extracted by ASPEC using extraction column( Pro Elut C_(18)500 mg/6 m L), dried by Turbo VapⅡ and dissolved in mobile phase. The supernatant was separated on Agilent SB-C_(18) column( 2. 1 mm × 50 mm, 1. 8 μm)using 0. 02 mmol/L ammonium acetate/methyle alcohol as mobile phase and then detected by HPLC-MS/MS using multiple reaction monitoring( MRM) in positive ionization and negative ionization mode.
The average recoveries were from 72. 6% to 100. 5%and the relative standard deviations( RSD) were from 0. 3% to 3. 1%( n = 6). The calibration curves showed a good linearity with correlation coefficients r > 0. 9990. The linear range for saccharin sodium was 8-800 μg/L and others were 2-200 μg/L. The detection limits for caffeine, benzoic acid, sorbic acid, acesulfame potassium and sodium cyclamate were 0. 001 mg/kg and 0. 004 mg/kg for saccharin sodium.
The method is specific, sensitive, easy, fast and suitable for the confirmation and quantification of caffeine, benzoic acid, sorbic acid, acesulfame potassium, saccharinsodium and sodium cyclamate in drink.
建立高效液相色谱-串联质谱法（HPLC-MS/MS）同时测定饮料中咖啡因、苯甲酸、山梨酸、安赛蜜、糖精钠和甜蜜素的方法。
采用ASPEC利用萃取柱（Pro Elut C₁₈ 500mg/6mL）对样品进行萃取，经Turbo VapⅡ吹干后用流动相溶解。上清液在Agilent SB-C₁₈柱（2.1mm×50mm，1.8μm）上以0.02mmol/L醋酸铵/甲醇为流动相进行分离，然后采用HPLC-MS/MS在正离子和负离子模式下通过多反应监测（MRM）进行检测。
平均回收率为72.6%至100.5%，相对标准偏差（RSD）为0.3%至3.1%（n = 6）。校准曲线线性良好，相关系数r＞0.9990。糖精钠的线性范围为8 - 800μg/L，其他为2 - 200μg/L。咖啡因、苯甲酸、山梨酸、安赛蜜和甜蜜素的检测限为0.001mg/kg，糖精钠的检测限为0.004mg/kg。
该方法特异性强、灵敏度高、简便快速，适用于饮料中咖啡因、苯甲酸、山梨酸、安赛蜜、糖精钠和甜蜜素的定性和定量分析。
