首页|高效液相色谱法测定硝酸甘油气雾剂定量阀门中5种抗氧剂含量与迁移量研究

高效液相色谱法测定硝酸甘油气雾剂定量阀门中5种抗氧剂含量与迁移量研究

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目的 建立同时测定硝酸甘油气雾剂定量阀门中 5 种常见抗氧剂含量的高效液相色谱(HPLC)法,并考察抗氧剂在其中的迁移情况。方法 色谱柱为Inertsil®ODS-SP柱(150 mm×4。6 mm,5µm),流动相为水-四氢呋喃-乙腈(10∶30∶60,V/V/V),流速为1。5 mL/min,柱温为 30℃,检测波长为 280 nm,进样量为 20µL。结果 抗氧剂 168、抗氧剂 330、抗氧剂 1010、抗氧剂 1076、抗氧剂2,6-二叔丁基对甲酚(BHT)的质量浓度均在 0。2~250µg/mL范围内与峰面积线性关系良好(r≥0。999 8,n=6);检测限分别为1。58,0。27,0。38,0。94,0。24µg/mL;定量限分别为 3。84,0。91,1。44,3。02,0。60µg/mL;精密度、稳定性、重复性试验结果的RSD均小于 2。0%(n=6);回收率分别为 100。67%,99。97%,99。93%,99。60%,99。63%,RSD分别为 0。47%,0。21%,0。93%,0。44%,0。60%(n=9)。硝酸甘油气雾剂定量阀门组件材料(内垫圈、阀杆、阀室、吸管)中抗氧剂 168、抗氧剂 330、抗氧剂 1010、抗氧剂 1076 的检出量均低于其评价阈值(AET),均未检出抗氧剂BHT。加速试验 0 个月、3 个月、6 个月,定量阀门组件材料中抗氧剂 168、抗氧剂 330、抗氧剂 1010、抗氧剂 1076、抗氧剂BHT的迁移量均低于其AET。结论 该方法操作简单、灵敏度高、结果准确、重复性和稳定性均较好,可用于硝酸甘油气雾剂定量阀门中 5 种抗氧剂的含量测定及迁移量研究。
Determination of Content and Migration of Five Antioxidants in Quantitative Valve of Nitroglycerin Aerosol by HPLC
Objective To establish a high-performance liquid chromatography(HPLC)method for the simultaneous determination of five antioxidants in quantitative valves of nitroglycerin aerosol,and to investigate the migration of antioxidants in nitroglycerin aerosols.Methods The chromatographic column was Inertsil®ODS-SP column(150 mm×4.6 mm,5 µm),the mobile phase was water-tetrahydrofuran-acetonitrile(10∶30∶60,V/V/V),the flow rate was 1.5 mL/min,the column temperature was 30℃,the detection wavelength was 280 nm,and the injection volume was 20 µL.Results The linear ranges of antioxidants 168,330,1010,1076,BHT were 0.2-250 µg/mL(r≥0.999 8,n=6),the limits of detection(LOD)were 1.58,0.27,0.38,0.94,0.24 µg/mL,the limits of quantification(LOQ)were 3.84,0.91,1.44,3.02,0.60 µg/mL.The RSDs of precision,stability,and repeatability test results were all lower than 2.0%(n=6).The recovery rates of the above five antioxidants were 100.67%,99.97%,99.93%,99.60%,and 99.63%,with RSDs of 0.47%,0.21%,0.93%,0.44%,and 0.60%(n=9),respectively.The detection levels of antioxidants 168,330,1010,1076 in the component materials such as the internal gasket,valve stem,valve chamber,and pipette of the quantitative valve of nitroglycerin aerosol were lower than those of corresponding analytical evaluation threshold(AET),and no antioxidant BHT was detected.After 0,3,and 6 months of accelerated tests,the migration volumes of antioxidants 168,330,1010,1076,and BHT in the component materials of the quantitative valve were all lower than those of corresponding AET.Conclusion This method is simple,highly sensitive,and accurate,with good repeatability and stability,which can be used for the determination of the content and migration of five antioxidants in quantitative valves of nitroglycerin aerosol.

nitroglycerin aerosolquantitative valveantioxidantcontent determinationmigration

肖海文、雷春华、林文辉

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湛江市明德医药科技有限公司,广东 湛江 524018

国家中药现代化工程技术研究中心 岭南药用芳香油分中心,广东 湛江 524017

广东同德药业有限公司,广东 湛江 524017

硝酸甘油气雾剂 定量阀门 抗氧剂 含量测定 迁移量

2024

中国药业
重庆市食品药品监督管理局

中国药业

CSTPCD
影响因子:1.369
ISSN:1006-4931
年,卷(期):2024.33(11)
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