Ling Yun, Chu Xiaogang, Zhang Feng, Chen Qi, Zhao Yunfeng, Wu Yongning, Zhang Chenguang
Chinese Centre for Disease Control and Prevention, Beijing 100021, China.
Se Pu. 2011 Aug;29(8):723-30.
An ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed for the simultaneous determination of 11 preservatives and 6 antioxidants in condiments. The condiment sample with low fat or middle fat was diluted with saturated NaCl solution (adjusting pH to 2 - 3 with phosphoric acid), then extracted with acetonitrile. The extract was purified using liquid-liquid extraction with hexane, and the sample with middle fat was further purified using solid phase extraction with a C8 column. The condiment sample with high fat was diluted with hexane, then dissolved with saturated NaCl solution (adjusting pH to 2 -3 with phosphoric acid), and extracted with acetonitrile. The extract was purified using solid phase extraction with a C8 column. The analysis was performed on a C18 column (150 mm x 2.1 mm, 1.7 microm) using a gradient elution with the mobile phases of 20 mmol/L ammonium acetate buffer and acetonitrile, and determined by tandem mass spectrometry in negtive ESI mode under multiple reaction monitoring (MRM) mode. The method had good linearity (r > or = 0.995 5). The limits of quantification (LOQs) (S/N = 10) of 17 analytes ranged from 0.05 mg/kg to 5 mg/kg. The recoveries ranged from 79.7% to 118% at three spiked levels, the relative standard deviations (RSDs) ranged from 0.57% to 13.1%. The method can be applied for the determination of preservatives and antioxidants in condiments.
建立了一种超高效液相色谱-电喷雾电离串联质谱法（UPLC-ESI-MS/MS），用于同时测定调味品中的11种防腐剂和6种抗氧化剂。低脂或中脂调味品样品用饱和氯化钠溶液稀释（用磷酸调节pH至2 - 3），然后用乙腈萃取。萃取液用正己烷液液萃取进行净化，中脂样品再用C8柱固相萃取进一步净化。高脂调味品样品用正己烷稀释，然后用饱和氯化钠溶液溶解（用磷酸调节pH至2 - 3），并用乙腈萃取。萃取液用C8柱固相萃取进行净化。采用C18柱（150 mm×2.1 mm，1.7μm），以20 mmol/L醋酸铵缓冲液和乙腈为流动相进行梯度洗脱，在负离子电喷雾电离模式下采用多反应监测（MRM）模式进行串联质谱测定。该方法具有良好的线性（r≥0.995 5）。17种分析物的定量限（LOQs）（S/N = 10）为0.05 mg/kg至5 mg/kg。在三个加标水平下回收率为79.7%至118%，相对标准偏差（RSDs）为0.57%至13.1%。该方法可用于测定调味品中的防腐剂和抗氧化剂。
