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目的建立超高效液相色谱-三重四级杆串联质谱测定火锅底料中吗啡、可待因、罂粟碱、那可汀、蒂巴因含量的方法。方法样品用1%三氯乙酸提取,提取液过固相萃取柱,用5%氨水-甲醇洗脱,洗脱液用氮吹浓缩仪吹至近干,用1 ml初始流动相复溶,以C_(18)柱分离,高效液相色谱-三重四级杆串联质谱仪测定,外标法定量。结果通过对仪器各项参数进行优化,有效克服了各种干扰的影响,方法精密度、线性范围及回归系数等各项指标均符合标准要求,方法检出限为0.2μg/kg,相关系数均大于0.999,其加标回收率在62.8%~106.0%之间,重复测定的相对标准偏差(RSD)为≤9.6%。结论该方法样品前处理简单,提取溶剂用量少,操作时间短,样品分析效率高,可广泛适用于火锅汤料、调料、酱料中罂粟壳类生物碱成分的测定。
OBJECTIVE To establish a method for the determination of morphine, codeine, papaverine, naltrexine and thebaine in hot pot bottom by ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry. Methods The sample was extracted with 1% trichloroacetic acid and the extract was passed through a solid-phase extraction column and eluted with 5% ammonia-methanol. The eluate was blown to near dryness with a nitrogen blow-off concentrator and reconstituted with 1 ml of the initial mobile phase. (18) column separation, high performance liquid chromatography - triple quadrupole mass spectrometry, external standard method. Results The parameters of the instrument were optimized to effectively overcome the effects of various disturbances. The methods such as precision, linearity range and regression coefficients were in accordance with the requirements of the standard. The detection limit was 0.2 μg / kg and the correlation coefficient Greater than 0.999, the spiked recoveries ranged from 62.8% to 106.0%, and the relative standard deviations (RSDs) of repeated determinations were ≤9.6%. Conclusion The method has simple pretreatment, less solvent extraction, short operation time and high sample analysis efficiency. It can be widely applied to the determination of opium poppy shell alkaloids in hotpot soups, spices and sauces.