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目的:建立药用明胶空心胶囊样品中22种合成色素的超高效液相色谱/三重四极杆质谱定量分析方法。方法:样品经60℃水、乙醇-水(7∶3)及乙腈浸泡超声提取,提取液采用聚酰胺粉吸附,固相萃取柱净化,分别以无水乙醇-水(3∶7)、无水乙醇-2%氨水-水(7∶2∶1)、乙腈解吸附,洗至聚酰胺粉无色;收集解吸液,旋蒸浓缩,加50%乙腈定容,经0.22μm滤膜过滤,进样分析。结果:10种限用色素线性浓度范围为5~500 mg·L~(-1),12种禁用色素的线性浓度范围为0.002~12.5 mg·L~(-1);22种合成色素均得到有效提取,加标提取回收率为72.1%~100.3%,检出限为0.5~284μg·L~(-1);146批次样品中,GB2760-2014规定允许作为食品添加剂使用的11种合成色素中,共检出8种,分别为柠檬黄、亮蓝、胭脂红、赤藓红、苋菜红、诱惑红、日落黄、喹啉黄,其中柠檬黄与亮蓝使用频率较高;禁用的合成色素中,15批次样品检出坚牢绿。结论:该方法对药用明胶空心胶囊中合成色素的定量分析有良好的适用性。采用建立方法,对多家企业产品进行测定,发现合成色素存在滥用现象,鉴于合成色素的危害性,其在制药工业中的使用品种、使用限量和安全性评价以及标签标示管理等方面应引起重视。
OBJECTIVE: To establish a method for the quantitative analysis of 22 synthetic pigments in pharmaceutical gelatin hollow capsules by ultra performance liquid chromatography / triple quadrupole mass spectrometry. Methods: The samples were extracted with 60 ℃ water, ethanol - water (7: 3) and acetonitrile soaking. The extracts were purified by polyamide powder and purified by solid phase extraction. The samples were eluted with absolute ethanol - water Water ethanol (7: 2: 1), desorption of acetonitrile, washing until the polyamide powder is colorless; collecting the desorption solution, concentrating by rotation, adding 50% acetonitrile to volume, filtering through a 0.22 μm membrane filter, Injection analysis. Results: The linear range of the 10 limiting pigments ranged from 5 to 500 mg · L -1. The linear range of the 12 prohibited dyes ranged from 0.002 to 12.5 mg · L -1. All 22 synthetic pigments were obtained The detection limit was 0.5 ~ 284μg · L -1. Of 146 batches of samples, GB2760-2014 regulated 11 kinds of synthetic pigments which were allowed to be used as food additives Among them, 8 kinds were detected, which were lemon yellow, brilliant blue, carmine, erythrosine, amaranth, temptation red, sunset yellow and quinoline yellow, of which lemon yellow and brilliant blue were used more frequently. Pigment, 15 batches of samples detected fast green. Conclusion: This method has good applicability to the quantitative analysis of synthetic pigment in medical gelatin hollow capsules. The establishment method was used to measure the products of many enterprises and found that there was a phenomenon of abuse of synthetic pigments. In view of the harmfulness of synthetic pigments, it should pay attention to such aspects as varieties used in the pharmaceutical industry, evaluation of usage limits and safety, and label labeling management .