超高效液相色谱-四极杆-飞行时间质谱测定果蔬中维生素C

doi:10.3724/SP.J.1123.2016.07015

色谱 ›› 2016, Vol. 34 ›› Issue (11): 1048-1054.DOI: 10.3724/SP.J.1123.2016.07015

超高效液相色谱-四极杆-飞行时间质谱测定果蔬中维生素C

刘真真^1,2, 齐沛沛², 王新全², 陈文学¹, 吴莉宇², 王强^1,2

1. 海南大学食品学院, 海南海口 570228;
2. 浙江省农业科学院农产品质量标准研究所, 浙江杭州 310021

收稿日期:2016-07-13 出版日期:2016-11-08 发布日期:2016-11-03
通讯作者: 王强
基金资助:
国家自然科学基金项目（31501556）；浙江省自然科学基金项目（LQ15B050001）；公益性行业（农业）科技专项（201503107）.

Determination of vitamin C in fruits and vegetables by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry

LIU Zhenzhen^1,2, QI Peipei², WANG Xinquan², CHEN Wenxue¹, WU Liyu², WANG Qiang^1,2

1. Food College, Hainan University, Haikou 570228, China;
2. Institute of Quality and Standard of Agro-Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021, China

Received:2016-07-13 Online:2016-11-08 Published:2016-11-03
Supported by:
National Natural Science Foundation of China (No. 31501556); Zhejiang Provincial Natural Science Foundation of China (No. LQ15B050001); Special Fund for Agro-Scientific Research in the Public Interest (No. 201503107).

摘要/Abstract

摘要：

利用超高效液相色谱-四极杆-飞行时间质谱（UPLC-Q-TOF/MS）快速与高分辨的分析优势，通过系统地考察样品制备、仪器分析中影响维生素C响应灵敏度和稳定性的各主要因素，建立了果蔬中维生素C的定量分析方法。果蔬样品在干冰保护下高速匀浆获得均匀的匀浆液，用0.1%（v/v）甲酸溶液提取后，采用Waters Acquity-UPLC T3色谱柱（100 mm×2.1 mm，1.8 μm）分析，柱温为30℃，进样量为5 μL，流动相为0.05%（v/v）甲酸-甲醇溶液（8：2，v/v），流速为0.25 mL/min。提取的定量离子为[M-H]^-（m/z 175.0238），定性离子为[M-C₃H₄O₃]^-（m/z 87.0077），质量允许误差为5×10^-6（5 ppm）。结果表明：维生素C在0.02~5.0 mg/L范围内峰面积与质量浓度呈线性，线性相关系数（R²）为0.9992；检出限及定量限分别为0.008 mg/L（S/N=3）和0.02 mg/L（S/N=10）；在不同添加水平下，维生素C的平均回收率为89.3%~113%，相对标准偏差小于5.40%。在优化的条件下，对32批次的国产和新西兰猕猴桃样品进行检测，国产猕猴桃中维生素C的含量范围为498~1625 mg/kg，新西兰进口猕猴桃中维生素C的含量范围为247~449 mg/kg。该方法操作简便，重复性良好，可用于果蔬中维生素C含量的准确测定。

关键词: 超高效液相色谱-四极杆-飞行时间质谱, 果蔬, 维生素C

Abstract:

A method was developed for the determination of vitamin C in fruits and vegetables by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry. The main factors which affect the sensitivity and stability of vitamin C in the sample preparation and instrument analysis were investigated. Fruit and vegetable samples were prepared by high speed homogenate under the protection of dry CO₂, and then extracted by 0.1% (v/v) formic acid solution. The analysis was performed using an Acquity-UPLC T3 column (100 mm×2.1 mm, 1.8 μm) with the column temperature of 30℃. The injection volume was 5 μL. The mobile phase consisted of 0.05% (v/v) formic acid solution and methanol with a volume ratio of 8:2. The flow rate was set at 0.25 mL/min. The extracted ion [M-H]^-(m/z 175.0238) was selected for quantification, while extracted ion [M-C₃H₄O₃]^-(m/z 87.0077) was selected for qualification. The mass error was 5×10^-6 (5 ppm). The results displayed that the linearity of vitamin C ranged from 0.02 to 5.0 mg/L with the correlation coefficient (R²) of 0.9992. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.008 mg/L (S/N=3) and 0.02 mg/L (S/N=10), respectively. The recoveries of the vitamin C in the spiked samples ranged from 89.3% to 113% with the RSD less than 5.40%. The developed method was then utilized to analyze the real kiwifruit samples. The results showed that the contents of the vitamin C ranged from 498 to 1625 mg/kg for the domestic kiwifruit samples. Regarding the New Zealand kiwifruit samples, the contents of the vitamin C ranged from 247 to 449 mg/kg. The present method demonstrated the advantages of easy operation, good precision and repeatability, making it feasible for accurate determination of vitamin C in fruits and vegetables.

Key words: fruits and vegetables, ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS), vitamin C

中图分类号:

O658

刘真真, 齐沛沛, 王新全, 陈文学, 吴莉宇, 王强. 超高效液相色谱-四极杆-飞行时间质谱测定果蔬中维生素C[J]. 色谱, 2016, 34(11): 1048-1054.

LIU Zhenzhen, QI Peipei, WANG Xinquan, CHEN Wenxue, WU Liyu, WANG Qiang. Determination of vitamin C in fruits and vegetables by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(11): 1048-1054.

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超高效液相色谱-四极杆-飞行时间质谱测定果蔬中维生素C

Determination of vitamin C in fruits and vegetables by ultra performance liquid chromatography-quadrupole time-of-flight mass spectrometry

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