液相色谱-四级杆-飞行时间质谱检测人参奶粉中的皂苷类成分

人参山羊奶粉是一种由人参超微粉与奶粉混合而成的乳制品,生产过程中常需要精确控制其中的皂苷成分。本文建立了一种人参奶粉中皂苷类成分的提取分离方法,并结合液相色谱-四级杆-飞行时间质谱(LC-Q-TOF-MS)技术对其中的皂苷单体成分进行了鉴定和定量分析。该提取方法回收率(101.1%~105.3%)和精密度(1.28%)高,稳定性好。通过二级质谱碎裂技术鉴定了奶粉中20种皂苷单体成分,并定量测定了Rg1,Re,Rb1,Rb2,Rc,Rd六种皂苷单体含量。干法制备的奶粉中总皂苷含量(3.44±0.51 mg/g)高于湿法制备获得的人参奶粉(2.38±0.14mg/g)。皂苷单体的测定结果与总皂苷一致,两种奶粉中皂苷单体的测定结果为:Rg1(11.22±3.1μg/g v.s. 8.03±2.9μg/g),Re (22.99±5.5μg/g v.s. 18.91±0.38μg/g),Rb1(7.43±0.41μg/g v.s. 4.83±0.14μg/g),Rb2(65.29±5.32μg/g v.s. 58.21±3.15μg/g),Rc(11.64±1.02μg/g v.s. 8.80±0.92μg/g),Rd(10.09±0.69μg/g v.s.7.81±0.52μg/g)。湿法制备得到的人参奶粉的均匀度较好,两种奶粉提取物中质谱检测未发现明显的皂苷降解峰。本方法可以为含有人参成分的食品分析检测和质量控制提供技术方案。

Determination of Ginseng Saponin in Ginseng-milk with Liquid Chromatography-Quadrupole-Time of Flight-mass Spectrometry

Ginseng goat milk powder is a dairy product made by mixing ginseng ultrafine powder with milk powder. An extraction and separation method was established and validated for the recovery, precision and stability. The liquid chromatography-Quadrupole-Time of Flight-mass spectrometry(LC-Q-TOF-MS) was used for the identification and quantification of saponin monomers. The method had good stability, high precision(1.28%) and high recovery(101.1-105.3%). Twenty saponin monomers were fingerprinted and identified with MS2, then the peak areas were compared in two milk powers. The content of saponin in ginseng milk powder obtained by dry preparation method(3.44±0.51 mg/g) was higher than that of ginseng milk powder obtained by wet preparation method(2.38±0.14 mg/g). However, the uniformity was poor. No obvious degradation components were found in the total ion chromatograms, which were consistent with total saponin results. Saponin monomers contents in two milk power were: Rg1(11.22±3.1 μg/g v.s. 8.03±2.9 μg/g), Re(22.99±5.5 μg/g v.s. 18.91±0.38 μg/g), Rb1 (7.43±0.41 μg/g v.s. 4.83±0.14 μg/g), Rb2(65.29±5.32 μg/g v.s. 58.21±3.15 μg/g), Rc(11.64±1.02 μg/g v.s. 8.80±0.92 μg/g), Rd(10.09±0.69 μg/g v.s.7.81±0.52 μg/g). The method can provide a basis for saponin detection in complex matrices in food field.