全自动QuEChERS-超高效液相色谱-串联质谱法快速测定辣椒粉中的氯酸盐及高氯酸盐

Rapid determination of chlorate and perchlorate in Capsicum annuum L. powder by automatic QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  全自动QuEChERS仪  氯酸盐及高氯酸盐  超高效液相色谱串联质谱法  辣椒粉

英文关键词:automatic QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  chlorate  perchlorate  Capsicum annuum L. powder

中文摘要:

      目的 建立全自动QuEChERS前处理结合超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)快速测定辣椒粉中氯酸盐和高氯酸盐的检测方法。方法 样品经集中称量后, 用1%乙酸乙腈-水(1:1, V:V)作为提取溶剂, 利用全自动QuEChERS仪编程后自动前处理, 采用0.5%甲酸甲醇-0.5%甲酸水溶液为流动相, Thermo HYPERCARB为分离柱, 进行梯度洗脱, 串联质谱电喷雾电离源负模式电离, 多反应离子监测模式检测, 以子离子比和保留时间定性, 用内标法定量。结果 采用全自动QuEChERS仪来进行辣椒粉氯酸盐及高氯酸盐的测定前处理效率是人工的6倍, 定量限(S/N=10)为10.0 μg/kg, 加标水平为10~50 μg/kg (n=6)时, 平均回收率为94.0%~96.4%, 相对标准偏差小于5%, 在1~100 μg/L范围内线性关系良好, 相关系数均大于0.999。结论 本方法自动化程度高、准确性及稳定性好, 同时定量限也满足欧盟出口的要求, 适用于出口辣椒粉中氯酸盐及高氯酸盐的测定。

英文摘要:

      Objective To establish a detection method for rapid determination of chlorate and perchlorate in Capsicum annuum L. powder by automatic QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the sample was centrally weighed, the sample was extracted with a mix-ture of 1% avetic acid-acetonitrile-water (1:1, V:V), and automatic pre-treatment with automatic QuEChERS instrument, the gradient elution was performed by 0.5% formic acid methanol-0.5% formic acid solution, Thermo HYPERCARB as a separation column, gradient elution, series mass spectra electrospray ionization negative mode ionization, multiresponse monitoring pattern detection, qualitative research by the ratio of retention time and ion, the internal standard method was used to qualitative experiment. Results Automatic QuEChERS instrument was used to determine the chlorate and perchlorate of Capsicum annuum L. powder and the pretreatment efficiency was 6 times that of manual. The limits of quantification (S/N=10) were 10 μg/kg, when the spiked level was 10–50 μg/kg (n=6), the sample recoveries for chlorate and perchlorate were 94.0%–96.4%, the relative standard deviations were less than 5%. The calibration curves were linear in the range of 1–100 μg/L with the correlation coefficients above 0.999. Conclusion The method has high automation degree, good accuracy and stability, and the limit of quantitation also meets the requirements of European Union export, can be applied for the determination of chlorate and perchlorate in Capsicum annuum L. powder.