高效液相色谱法同时测定棉籽油中游离棉酚及其降解产物四甲氧基棉酚含量

doi:10.7506/spkx1002-6630-20180926-282

食品科学 ›› 2019, Vol. 40 ›› Issue (16): 261-266.doi: 10.7506/spkx1002-6630-20180926-282

高效液相色谱法同时测定棉籽油中游离棉酚及其降解产物四甲氧基棉酚含量

周梦宇，古丽斯坦·阿不来提，姚军，陈玲

新疆医科大学药学院，新疆乌鲁木齐 830011

出版日期:2019-08-25 发布日期:2019-08-26
基金资助:
国家自然科学基金地区科学基金项目（31460417）；新疆维吾尔自治区高校科研计划自然科学重点项目（XJEDU2018I012）

Simultaneous Determination of Free Gossypol and Its Degradation Product Tetramethoxy Gossypol in Commercially Available Cottonseed Oil by High Performance Liquid Chromatography

ZHOU Mengyu, Gulisitan·ABULAITI, YAO Jun, CHEN Ling

College of Pharmacy, Xinjiang Medical University, ürümqi 830011, China

Online:2019-08-25 Published:2019-08-26

摘要/Abstract

摘要： 建立高效液相色谱法测定市售棉籽油中游离棉酚及其降解产物四甲氧基棉酚的含量方法，为棉籽油质量控制提供科学依据。采用Inertsil? ODS-3（250 mm×4.6 mm，5 mm）色谱柱，以甲醇-2%磷酸（85∶15，V/V）溶液为流动相，流速1.0 mL/min，柱温32 ℃，检测波长235 nm，进样量10 mL。棉酚在0.245～1.226 mg/mL质量浓度范围内线性关系良好（r=0.999 5），精密度检测相对标准偏差为0.88%（n=6），重复性检测相对标准偏差为1.73%（n=6），平均回收率为101.2%，相对标准偏差为1.75%（n=3）。四甲氧基棉酚在0.211～1.056 mg/mL质量浓度范围内线性关系良好（r=0.999 6），精密度检测相对标准偏差为1.56%（n=6），重复性检测相对标准偏差为1.11%（n=6），平均回收率为100.3%，相对标准偏差为1.12%（n=3）。90 批市售棉籽油中有25 批检测到棉酚，且质量浓度为0.159～1.661 mg/mL，有56 批检测到四甲氧基棉酚，且质量浓度为0.093～1.661 mg/mL。该法有良好的准确度、精密度，操作简便，可较广泛用于监控棉籽油的脱毒情况。

关键词: 高效液相色谱法, 游离棉酚, 四甲氧基棉酚, 含量测定

Abstract: This study aimed to establish a high performance liquid chromatography (HPLC) method for the determination of free gossypol and its degradation product tetramethoxy gossypol in commercially available cottonseed oil in order to provide a scientific basis for quality control of cottonseed oil. The chromatographic separation was accomplished on an Inertsil? ODS-3 column (250 mm × 4.6 mm, 5 mm) using a mobile phase comprised of methanol and 2% phosphoric acid (85:15, V/V) at a flow rate of 1.0 mL/min, and the column temperature was set at 32 ℃. The detection wavelength was 235 nm, and the injection volume was 10 mL. Good linear relationship was achieved for gossypol in the concentration range of 0.245–1.226 mg/mL (r = 0.999 5). The relative standard deviation (RSD) of precision and repeatability was 0.88% and 1.73% (n = 6), respectively. The average recovery was 101.2%, with RSD of 1.75% (n = 3). The method also showed a good linear relationship for tetramethoxy gossypol in the concentration range of 0.211–1.056 mg/mL (r = 0.999 6). The RSD of precision and repeatability was 1.56% and 1.11% (n = 6), respectively. The average recovery was 100.3%, with RSD of 1.12% (n = 3). Free gossypol was detected in 25 out of 90 batches of commercially available cottonseed oils in the range of 0.159– 1.661 mg/mL, and tetramethoxy gossypol in 56 in the range of 0.093–1.661 mg/mL. This method displayed good accuracy, high precision and easy operation and could be widely used to monitor the detoxification of cottonseed oil.

Key words: high performance liquid chromatography, free gossypol, tetramethoxy gossypol, determination

中图分类号:

TS22

周梦宇，古丽斯坦·阿不来提，姚军，陈玲. 高效液相色谱法同时测定棉籽油中游离棉酚及其降解产物四甲氧基棉酚含量[J]. 食品科学, 2019, 40(16): 261-266.

ZHOU Mengyu, Gulisitan·ABULAITI, YAO Jun, CHEN Ling. Simultaneous Determination of Free Gossypol and Its Degradation Product Tetramethoxy Gossypol in Commercially Available Cottonseed Oil by High Performance Liquid Chromatography[J]. FOOD SCIENCE, 2019, 40(16): 261-266.

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高效液相色谱法同时测定棉籽油中游离棉酚及其降解产物四甲氧基棉酚含量

Simultaneous Determination of Free Gossypol and Its Degradation Product Tetramethoxy Gossypol in Commercially Available Cottonseed Oil by High Performance Liquid Chromatography

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