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目的:建立棉籽仁、棉叶及棉茎中游离棉酚含量的LC-MS内标检测法。方法:以甘草次酸为内标物,采用YMC-C18色谱柱(150 mm×3.0 mm,3μm),流动相为乙腈:1%甲酸溶液=80:20,流速0.3 mL/min,柱温25℃;电喷雾离子源(ESI),负离子模式,选择性离子监测(SIM),棉酚的检测离子为[M-H]-,m/z 516.6,内标甘草次酸的检测离子为[M-H]-,m/z 468.9。结果:棉酚质量浓度在1.008~50.40μg/mL范围内呈良好线性关系,加标回收率为90.3%~103.6%,RSD为1.8%~3.7%。结论:该方法灵敏度高、专属性强,样品处理简便易行,可准确测定棉籽仁、棉叶和棉茎中棉酚的含量。
Objective: To establish a LC-MS method for the determination of free gossypol in cottonseed kernels, cotton leaves and cotton stems. Methods: YMC-C18 column (150 mm × 3.0 mm, 3 μm) was used with glycyrrhetic acid as internal standard. The mobile phase consisted of acetonitrile: 1% formic acid solution 80:20, flow rate 0.3 mL / ℃; electrospray ionization (ESI), negative ion mode, selective ion monitoring (SIM), the detection ion of gossypol is [MH] -, m / z 516.6, , m / z 468.9. Results: There was a good linear relationship between the concentration of gossypol and 1.008 ~ 50.40μg / mL. The spiked recoveries ranged from 90.3% to 103.6% with RSD ranging from 1.8% to 3.7%. Conclusion: The method is sensitive, specific and easy to handle. It can accurately determine the content of gossypol in cottonseed kernels, cotton leaves and cotton stems.