采用提取和净化相结合的前处理方式,建立并优化了同时测定蛋白饮料、液体调味品中36种防腐剂的超高效液相色谱-串联质谱检测方法。样品采用饱和NaCl溶液(用磷酸调节pH=3)净化和乙腈-甲醇(9∶1,体积比)(含体积分数为0.2%的甲酸)提取。采用C18反向色谱柱进行分离,以甲醇和5 mmol/L乙酸铵为流动相梯度洗脱,采用电喷雾离子源正负离子同时扫描,动态多反应监测模式,基质匹配标准曲线,外标法定量。结果表明,36种防腐剂在1～250 ng/mL线性良好(相关系数≥0.999),方法定量限为0.04～0.2 mg/kg;空白样品不同加标水平下的平均加标回收率为75%～119%;相对标准偏差为0.90%～9.8%。建立的高通量检测方法灵敏、快速,准确度高,操作简便且能有效减少基质干扰、降低检测成本,极大提高多种防腐剂的定性定量检测效率。
An ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-MS/MS) method was developed and optimized for the simultaneous determination of 36 preservatives in protein drinks and liquid condiments by the pretreatment method of combining extraction and purification. The samples were purified with saturated sodium chloride solution (adjusting pH to 3 with phosphoric acid) and extracted with acetonitrile-methanol (9∶1, volume ratio) (containing 0.2% formic acid). The analytes were separated on a C18 chromatographic column using gradient elution with methanol-5 mmol/L ammonium acetate as the mobile phase, detected by MS/MS in both positive ion and negative ion mode using dynamic multiple reaction monitoring, and finally quantified by the matrix-matched external standard method. Results showed that good linearity was observed for the 36 compounds with correlation coefficients≥0.999 in the concentration range of 1-250 ng/mL, and the limits of quantitation were between 0.04 mg/kg and 0.2 mg/kg. The average recoveries of blank samples were in the range of 75%-119%, with relative standard deviations of 0.90%-9.8%. The established high-throughput detection method is sensitive, rapid, accurate, and simple, can effectively reduce matrix interference, reduce detection cost, shorten the detection cycle, and greatly improve the qualitative and quantitative detection efficiency of various preservatives.
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