超高效液相色谱-串联质谱法同时分析紫薯中15种酚酸类组分

刘文静; 黄彪; 林香信; 方灵; 吴建鸿; 李巍; 吴妙鸿

doi:10.19303/j.issn.1008-0384.2019.10.014

超高效液相色谱-串联质谱法同时分析紫薯中15种酚酸类组分

Simultaneous Determination of 15 Phenolic Compounds in Purple Potato by High Performance Liquid Chromatography-tandem Mass Spectrometry

摘要

摘要:
目的运用超高效液相色谱-串联质谱（UPLC-MS/MS）分析不同品种紫薯中酚酸类组分及含量，为紫薯中酚酸类组分的提取、分析提供理论依据。
方法建立超高效液相色谱-串联质谱法同时检测紫薯中15种酚酸类组分的方法，分析8种不同品种紫薯中酚酸类组分的含量。样品经甲醇-水溶液超声提取后，使用Waters T3 C₁₈色谱柱(250 mm × 4.6 mm，5 μm)，以0.1%（v/v）甲酸-5 mmol·L⁻¹乙酸铵水溶液和乙腈为流动相进行梯度洗脱，负离子扫描方式下多反应监测(MRM)模式测定。
结果在优化的试验条件下，15种酚酸类组分在相应的浓度范围内具有良好的线性关系，相关系数（r）为0.995 6～0.999 7，方法检出限和定量限分别为0.3～5.8 μg·L⁻¹(S/N ≥3)和1.0～15.2 μg·L⁻¹(S/N ≥10)；加标试验平均回收率73.3%～97.1%，相对标准偏差1.8%～8.9%。
结论在所分析的紫薯样品中共检出5种酚酸类组分，含量0.102～1 698.490 mg·kg⁻¹，其中绿原酸含量最高，对香豆酸含量最低。该法灵敏、快速、准确，适用于紫薯中酚酸类组分的定性定量分析。

Abstract:
Objective A method coupling the ultra-high performance liquid chromatography and the triple-quadrupole tandem mass spectrometry (UPLC-MS/MS) was established to simultaneously determine 15 phenolic compounds in purple potatoes.
Method Purple potato specimens were extracted with methanol-water under ultrasound to be separated on a UPLC and analyzed by MS/MS for the phenolic determination. On a Waters T3 C₁₈ column of the UPLC, the extracts was separated by gradient elution with 0.1% (V/V) formic acid-5 mmol·L⁻¹ammonium acetate aqueous solution and acetonitrile as the mobile phase. The elutes were analyzed using the positive electrospray ionization tandem MS under the multiple reaction monitoring mode.
Result With the optimized conditions and within the concentration range, linearities on the measurements for 15 phenolics with correlation coefficients ranging from 0.995 6 to 0.999 7 were obtained. The methodology had a limit of detection (LOD) of 0.3–5.8 µg·L⁻¹ (S/N≥3) and that of quantitation 1.0–15.2 µg·L⁻¹ (S/N≥10). The average recoveries on the compounds ranged from 73.3% to 97.1% with a relative standard deviation (RSDs) of 1.8%–8.9%.
Conclusion Five categories of phenolic compounds in the concentrations ranging from 0.102 mg·kg⁻¹ to 1 698 490 mg·kg⁻¹ were detected in the purple potato specimens by the method. Among them, chlorogenic acid was the highest in quantity, and coumaric acid the lowest. The newly established methodology was deemed sensitive, rapid, accurate, and suitable for phenolic determination on purple potatoes.

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