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建立了花粉中链霉素(streptomycin,STR)与双氢链霉素(dihydrostreptomycin,DHS)的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经提取液提取、三氯甲烷沉淀蛋白后,用C18固相萃取柱进行富集净化,采用HPLC-MS/MS对目标物进行定性确证和定量分析。在Protemix WCX-NP5色谱柱(100 mm×2.1 mm,5μm)上以5%(v/v)甲酸、20 mmol/L醋酸铵和甲醇为流动相进行梯度洗脱分离;质谱采集模式为电喷雾正离子监测模式。链霉素和双氢链霉素的检出限(以信噪比(S/N)=3计)均为5μg/kg,定量限(以S/N=10计)均为10μg/kg;在10~200μg/L的质量浓度范围内呈现良好的线性关系,相关系数(r)大于0.99。本底空白的松花粉、玉米花粉、茶花粉、葵花粉、油菜花粉、杂花粉等6种基质中10、20、50μg/kg添加水平下的加标回收率范围为76.8%~100.3%,精密度范围为3.70%~12.6%。该方法无需使用对LC-MS联用仪容易造成污染的七氟正丁酸,且方法准确可靠,适用于大部分花粉基质的测定。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) method was developed for the determination of streptomycin (STR) and dihydrostreptomycin (DHS) in pollen. The sample was extracted with the extract and the protein was precipitated with trichloromethane. The sample was concentrated and purified with a C18 solid-phase extraction column. The qualitative and quantitative analysis of the target substance was carried out by HPLC-MS / MS. The separation was performed on a Protemix WCX-NP5 column (100 mm × 2.1 mm, 5 μm) using a gradient elution with 5% (v / v) formic acid, 20 mmol / L ammonium acetate and methanol as the mobile phase. Positive ion monitoring mode. The detection limit of streptomycin and dihydrostreptomycin (S / N = 3) was 5μg / kg and the limit of quantitation (S / N = 10) was 10μg / kg. In the concentration range of 10 ~ 200μg / L showed a good linear relationship, the correlation coefficient (r) greater than 0.99. The spiked recoveries of blank maize, maize pollen, tea pollen, sunflower, rape pollen and heterosis in the blank medium ranged from 76.8% to 100.3% at the spiked levels of 10, 20 and 50 μg / Degrees range from 3.70% to 12.6%. This method does not require the use of heptafluoro-n-butyric acid, which is easily contaminated by LC-MS. The method is accurate and reliable and suitable for the determination of most pollen matrices.