CN110320293A - 一种测定苯酞类化合物中残留溶剂的方法 - Google Patents
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Abstract
Description
名称 | 丁苯酞称样量mg | 本底量ug | 加入量ug | 测得量ug | 回收率% |
正庚烷 | 1024.7 | 0 | 4995 | 3745 | 75.0 |
名称 | 丁苯酞称样量mg | 本底量ug | 加入量ug | 测得量ug | 回收率% |
正庚烷 | 1011.2 | 0 | 4866 | 3193 | 65.6 |
名称 | 丁苯酞称样量mg | 本底量ug | 加入量ug | 测得量ug | 回收率% |
正庚烷 | 1024.6 | 0 | 4906 | 4293 | 87.5 |
名称 | 甲醇 | 乙腈 | 二氯甲烷 | 乙酸乙酯 | 四氢呋喃 |
平均回收率% | 103.2 | 102.9 | 104.9 | 100.1 | 95.1 |
RSD% | 3.66 | 3.55 | 4.37 | 3.96 | 3.76 |
名称 | A-样1 | A-样2 | A-样3 | A-样4 | A-样5 | A-样6 | A平均 | RSD% |
甲醇 | 358.12 | 331.4 | 333.71 | 360.67 | 323.18 | 320.34 | 337.90 | 5.15 |
乙腈 | 69.55 | 63.96 | 64.21 | 69.74 | 61.66 | 61.58 | 65.12 | 5.65 |
二氯甲烷 | 50.58 | 45.5 | 46.6 | 50.63 | 44.65 | 43.75 | 46.95 | 6.35 |
乙酸乙酯 | 1427.56 | 1274.19 | 1309.58 | 1424.17 | 1258.68 | 1222.91 | 1319.52 | 6.59 |
四氢呋喃 | 381.67 | 340.78 | 352.02 | 381.29 | 338.72 | 327.5 | 353.66 | 6.48 |
正庚烷 | 10250.02 | 9141.65 | 9521.74 | 10213.49 | 9206.62 | 8793.86 | 9521.23 | 6.27 |
名称 | 甲醇% | 乙腈% | 二氯甲烷% | 乙酸乙酯% | 四氢呋喃% | 正庚烷% |
丁苯酞样品1 | 未检出 | 未检出 | 未检出 | 未检出 | 未检出 | 0.00007 |
丁苯酞样品2 | 未检出 | 未检出 | 未检出 | 0.003 | 未检出 | 0.0004 |
丁苯酞样品3 | 未检出 | 未检出 | 未检出 | 0.001 | 未检出 | 0.0001 |
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Cited By (12)
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CN111289654A (zh) * | 2020-03-19 | 2020-06-16 | 陕西省食品药品监督检验研究院 | 一种盐酸尼卡地平原料中甲醇、丙酮、三氯甲烷和甲苯四种残留溶剂的检测方法 |
CN111351874A (zh) * | 2020-03-16 | 2020-06-30 | 山东省药学科学院 | 一种异丁司特原料药中残留溶剂的检测方法 |
CN111855837A (zh) * | 2020-06-29 | 2020-10-30 | 武汉九州钰民医药科技有限公司 | 一种头孢噻肟钠中残留溶剂的检测方法及应用 |
CN112557531A (zh) * | 2020-11-27 | 2021-03-26 | 衢州康鹏化学有限公司 | 一种顶空气相色谱检测硫酸乙烯酯中残留溶剂的方法 |
CN112684044A (zh) * | 2020-12-17 | 2021-04-20 | 山东省药学科学院 | 一种拉帕替尼原料药中残留溶剂的检测方法 |
CN112730685A (zh) * | 2020-12-28 | 2021-04-30 | 浙江工业大学 | 一种乙酸乙酯和石油醚混合溶剂的回收与分析测试方法 |
CN112964813A (zh) * | 2019-12-13 | 2021-06-15 | 金陵药业股份有限公司 | 一种盐酸法舒地尔中有机溶剂残留量的测定方法 |
CN113607843A (zh) * | 2021-07-30 | 2021-11-05 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | 一种检测西罗莫司原料药中残留溶剂的方法 |
CN113960229A (zh) * | 2021-10-22 | 2022-01-21 | 云南中烟工业有限责任公司 | 一种烟用爆珠精油中甲醇含量的测定方法 |
CN114216992A (zh) * | 2021-12-27 | 2022-03-22 | 兰晟生物医药(苏州)有限公司 | 顶空气相色谱法测定左旋盐酸去甲基苯环壬酯中残留溶剂的方法 |
CN114965791A (zh) * | 2022-06-14 | 2022-08-30 | 江苏慧聚药业股份有限公司 | 一种顶空气相色谱法测定普乐沙福中残留的方法 |
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2009010806A1 (en) * | 2007-07-18 | 2009-01-22 | Generics [Uk] Limited | Assay methods for memantine |
CN104628649A (zh) * | 2015-01-23 | 2015-05-20 | 云南昊邦制药有限公司 | 一种2-(α-羟基戊基)苯甲酰胺衍生物及其制备方法、制剂与应用 |
CN105067724A (zh) * | 2015-08-05 | 2015-11-18 | 山东省药学科学院 | 一种检测新利司他中有机溶剂残留的方法 |
CN105806968A (zh) * | 2014-12-31 | 2016-07-27 | 江苏万邦生化医药股份有限公司 | 同时检测正庚烷、异辛烷、乙酸乙酯、异丙醇的气相色谱分析方法及其应用 |
CN106018631A (zh) * | 2016-08-16 | 2016-10-12 | 中国烟草总公司郑州烟草研究院 | 一种浸膏类添加剂溶剂残留的分析方法 |
CN107202841A (zh) * | 2017-05-24 | 2017-09-26 | 深圳天祥质量技术服务有限公司 | 涂料中degbe、degme和pgme含量的检测方法 |
CN109709219A (zh) * | 2017-10-25 | 2019-05-03 | 中国石油化工股份有限公司 | 检测非极性基质中极性物质结构和/或含量的方法 |
-
2019
- 2019-06-28 CN CN201910579722.XA patent/CN110320293B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2009010806A1 (en) * | 2007-07-18 | 2009-01-22 | Generics [Uk] Limited | Assay methods for memantine |
CN105806968A (zh) * | 2014-12-31 | 2016-07-27 | 江苏万邦生化医药股份有限公司 | 同时检测正庚烷、异辛烷、乙酸乙酯、异丙醇的气相色谱分析方法及其应用 |
CN104628649A (zh) * | 2015-01-23 | 2015-05-20 | 云南昊邦制药有限公司 | 一种2-(α-羟基戊基)苯甲酰胺衍生物及其制备方法、制剂与应用 |
CN105067724A (zh) * | 2015-08-05 | 2015-11-18 | 山东省药学科学院 | 一种检测新利司他中有机溶剂残留的方法 |
CN106018631A (zh) * | 2016-08-16 | 2016-10-12 | 中国烟草总公司郑州烟草研究院 | 一种浸膏类添加剂溶剂残留的分析方法 |
CN107202841A (zh) * | 2017-05-24 | 2017-09-26 | 深圳天祥质量技术服务有限公司 | 涂料中degbe、degme和pgme含量的检测方法 |
CN109709219A (zh) * | 2017-10-25 | 2019-05-03 | 中国石油化工股份有限公司 | 检测非极性基质中极性物质结构和/或含量的方法 |
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CN114216992A (zh) * | 2021-12-27 | 2022-03-22 | 兰晟生物医药(苏州)有限公司 | 顶空气相色谱法测定左旋盐酸去甲基苯环壬酯中残留溶剂的方法 |
CN115097027A (zh) * | 2022-06-08 | 2022-09-23 | 河北常山生化药业股份有限公司 | 枸橼酸西地那非原料药中残留溶剂的气相色谱检测方法 |
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