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复方丹参片检验方法确认方案

2018-01-08 21页 doc 61KB 10阅读

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复方丹参片检验方法确认方案复方丹参片检验方法确认方案 文件编号: 文件审定 部门 签名 日期 起草人 审核人 批准人 浙江优康制药有限公司 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extend...
复方丹参片检验方法确认方案
复方丹参片检验方法确认 文件编号: 文件审定 部门 签名 日期 起草人 审核人 批准人 浙江优康制药有限公司 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 1. 概述: 复方丹参片质量标准为已验证的法定标准,含量测定方法为HPLC法,其它项 目为实验室日常测试步骤。根据2010年版《药品质量管理》的要求,需 要对含量测定检验方法进行确认,包括专属性、精密度、准确度三个方面。 2. 目的: 确认复方丹参片含量测定检验方法在我公司质量控制实验室的适用性。 3. 适用范围: 复方丹参片含量测定检验方法 4. 条件: 4.1. 检验操作规程齐全 4.2. 设备相关标准操作规程齐全 4.3. 检验、检测仪器均已校验 5. 确认时间:从 年 月 日开始至 年 月 日完成。 6. 含量测定含丹参以丹参酮IIA计检测方法确认 6.1( 确认要求及标准 6.1.1. 色谱条件系统适用性试验(在专属性试验时一并进行):用十八烷基硅烷键合硅胶为填充剂;以甲醇-水-(73?27)为流动相;检测波长为270nm。理论板数以丹参酮IIA峰计算应不低于2000,分离度大于1.5。 6.1.2. 专属性 空白样品溶液在与丹参酮IIA对照品溶液相同的保留时间处色谱峰峰面积小于对照品峰面积的3%。 6.1.3. 精密度 RSD应不得超过2.0% 6.1.4. 准确度 丹参酮IIA的加样回收率98.0%,102%,回收率的RSD小于2.0%。 6.2. 材料和方法 6.2.1. 试剂: 对照品 :丹参酮IIA 批号 : 来源: 样品 :复方丹参片 批号 : 来源: 试剂名称:甲醇 批号 : 来源: 空白对照物:按复方丹参片质量标准制法自制(缺丹参) rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 6.2.2. 仪器: 高效液相色谱仪型号: 编号: 色谱柱编号: 分析天平型号 : 编号: 超声处理器型号: 编号: 6.2.3(溶液配置: 6.2.3.1.对照品溶液配置 取丹参酮IIA对照品适量,精密称定,置棕色量瓶中,加甲醇制成每1ml含40微克的溶液即得。 6.2.3.2供试品溶液 取复方丹参片20片,除去糖衣片,精密称定,研细, 取约1g,精密称定后置具塞棕色瓶中,精密加入甲醇25ml,密塞称定重量, 超声处理15分钟,放冷,再称定重量并补足,摇匀滤过取续滤液置棕色 瓶中即得。 6.2.3.3. 空白物溶液 取空白物20片,除去糖衣片,精密称定,研细, 取约1g,精密称定后置具塞棕色瓶中,精密加入甲醇25ml,密塞称定重量, 超声处理15分钟,放冷,再称定重量并补足,摇匀滤过取续滤液置棕色 瓶中即得。 6.2.3.4.储备液A 精密称取丹参酮IIA对照品适量,精密称定,置棕色量瓶中,加甲醇制成每1ml含120微克的溶液即得。 6.2.4 分析方法: 用十八烷基硅烷键合硅胶为填充剂;以甲醇-水-(73?27)为流动相;检测波长为270nm;进样量为10 ul。 6.3.检验方法的确认 6.3.1专属性 6.3.1.1 色谱条件与系统适用性试验 用十八烷基硅烷键合硅胶为填充剂;以甲醇-水-(73?27)为流动相;检测波长为270nm。理论丹参酮IIA峰计算应不低于2000,分离度大于1.5。 6.3.1.2. 测定 分别精密吸取对照品溶液与空白样品溶液各10µl,注入液相色谱仪,测定,记录色谱图。 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 6.3.1.3. 确认合格标准 空白样品溶液在与丹参酮IIA对照品溶液相同的保留 时间处色谱峰峰面积小于对照品峰面积的3%。 6.3.2.精密度 6.3.2.1重复性 6.3.2.1.1. 取同一浓度的对照品溶液及供试品溶液分别连续进样6针(10ul),记录色谱图。 6.3.2.1.2. 确认合格标准 6针对照品溶液、供试品溶液峰面积的RSD应不得超过2.0%。 6.3.2.2中间精密度 6.3.2.2.1. 在不同的日期和不同的仪器,不同检验员(3人)按6.2.3.2的方法重新制备样液,分别计算含量。 6.3.2.2.2. 确认合格标准 每人RSD应不得超过2.0%,3人RSD应不得超过2.0%。 6.3.3准确度 表1 溶液编号 加入储备液A加入空白对照容量瓶(ml) 进样浓度(ug (ml) 物(g) ,ml) 1 6.0 1 25 28.8 2 7.0 1 25 33.6 3 6.0 0.8 20 36 4 8.0 1 25 38.4 5 7.0 0.8 20 42 6 9.0 1 25 43.2 7 10.0 1 25 48 8 11.0 1 25 52.8 9 9.0 0.8 20 54 6.3.3.1溶液1,9:将表2中规定量的储备液A 和空白对照物置于规定量的具塞棕色容量瓶中,用甲醇补足至25ml,密塞称定重量,超声处理15分钟,放冷,rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 再称定重量并补足,摇匀滤过取续滤液置棕色瓶中即得。 6.3.3.2精密吸取9份样液各10ul,注入液相色谱仪,测定,计算回收率。 计算公式: 测得值 ×100% 回收率(%)= 加入的对照品量 6.3.3.3(确认合格标准 丹参酮IIA的加样回收率收率98.0%,102%,回收率的RSD小于2.0%。 7. 含量测定含丹参以丹酚酸B计检测方法确认 确认要求及标准 7.1( 7.1.1. 色谱条件系统适用性试验(在专属性试验时一并进行):用十八烷基硅烷键合硅胶为填充剂;以乙腈,甲醇,甲酸,水(10:30:1:59)为流动相;检测波长为286nm。理论板数以丹酚酸B峰计算应不低于4000。 7.1.2. 专属性 空白样品溶液在与丹酚酸B对照品溶液相同的保留时间处色谱峰峰面积小于对照品峰面积的3%。 7.1.3. 精密度 RSD应不得超过2.0% 7.1.4. 准确度 丹参酮IIA的加样回收率大于收率98.0%,102%,回收率的RSD小于2.0%。 7.2. 材料和分析方法 7.2.1. 试剂: 对照品 :丹参酮IIA 批号 : 来源: 样品 :复方丹参片 批号 : 来源: 试剂名称:乙腈 批号 : 来源: rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 试剂名称:甲酸 批号 : 来源: 试剂名称:甲醇 批号 : 来源: 空白对照物:按复方丹参片质量标准制法自制(缺丹参) 7.2.2. 仪器: 高效液相色谱仪型号: 编号: 色谱柱编号: 分析天平型号 : 编号: 超声处理器型号: 编号: 7.2.3(溶液配置: 7.2.3.1.对照品溶液配置 取丹酚酸B对照品适量,精密称定,加水制成每1ml含60微克的溶液即得。 7.2.3.2供试品溶液 取复方丹参片20片,除去糖衣片,精密称定,研细, 取约0.15g,精密称定后置50ml具塞量瓶中,加水适量,超声处理30分钟,放冷,加水至刻度,摇匀离心取上清夜即得。 7.2.3.3. 空白物溶液 取空白对照物20片,除去糖衣片,精密称定,研细, 取约0.15g,精密称定后置50ml具塞量瓶中,加水适量,超声处理30分钟,放冷,加水至刻度,摇匀离心取上清夜即得。 7.2.4 分析方法: 用十八烷基硅烷键合硅胶为填充剂;以乙腈,甲醇,甲酸,水(10:30:1:59)为流动相;检测波长为286nm;进样量为10 ul。 7.3.检验方法的确认 7.3.1专属性 7.3.1.1 色谱条件与系统适用性试验 用十八烷基硅烷键合硅胶为填充剂;以乙腈,甲醇,甲酸,水(10:30:1:59)为流动相;检测波长为286nm。理论板数以丹酚酸B峰计算应不低于4000。 7.3.1.2. 测定 分别精密吸取对照品溶液与空白样品溶液各10µl,注入液相色谱仪,测定,记录色谱图。 7.3.1.3. 确认合格标准 空白样品溶液在与丹酚酸B对照品溶液相同的保留间 处色谱峰峰面积小于对照品峰面积的3%。 7.3.2.精密度 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 7.3.2.1重复性 7.3.2.1.1. 取同一浓度的对照品溶液及供试品溶液分别连续进样6针(10ul),记录色谱图。 7.3.2.1.2. 确认合格标准 6针对照品溶液、供试品溶液峰面积的RSD应不得超过2.0%。 7.3.2.2中间精密度 7.3.2.2.1. 在不同的日期和不同的仪器,不同检验员(3人)按7.2.3.2的方法重新制备样液,分别计算含量。 7.3.2.2.2. 确认合格标准 每人RSD应不得超过2.0%,3人RSD应不得超过2.0%。 7.3.3准确度 7.3.3.1取丹酚酸B对照品适量,精密称定,置棕色量瓶中,加水制成每1ml含60微克的溶液。取上述(7.2.3.2)研细的复方丹参片样品0.09g,精密称定10份,分别置于50ml具塞量瓶中,并分别加入对照品溶液0、10、10、10、20、20、20、30、30、30ml,加入适量水超声处理30分钟,放冷后用水补足至刻度,摇匀离心取上清夜即得。 7.3.3.2精密吸取10份样液各10ul,注入液相色谱仪,测定,计算回收率。 计算公式: 测得值-样品中的量 ×100% 回收率(%)= 加入的对照品量 7.3.3.3(确认合格标准 丹酚酸B的加样回收率收率98.0%,102%,回收率的RSD小于2.0%。 8. 含量测定含三七以人参皂苷Rg、人参皂苷Rb、人参皂苷R、人参皂苷Re111计检测方法确认 8.1( 确认要求及标准 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 8.1.1. 色谱条件系统适用性试验(在专属性试验时一并进行):用十八烷基硅烷键合硅胶为填充剂;以乙腈为流动相A,以水为流动相B,按表1的规定进行梯度洗脱检测波长为203nm。理论板数以人参皂苷Rg峰计算应不低于6000,人1 参皂苷Rg与人参皂苷Re的分离度应大于1.8. 1 表2 时间(分钟) 流动相A(,) 流动相B(,) 19 81 0,35 35,55 19,29 81,71 29 71 55,70 70,100 29,40 71,60 8.1.2. 专属性 空白样品溶液在与对照品溶液相同的保留时间处色谱峰峰面积小于对照品峰面积的3%。 8.1.3. 精密度 RSD应不得超过2.0% 8.1.4. 准确度 参皂苷Rg、人参皂苷Rb、人参皂苷R、人参皂苷Re的加样111回收率大于收率98.0%,102%,回收率的RSD小于2.0%。 8.2. 材料和分析方法 8.2.1. 试剂: 对照品 :丹参酮IIA 批号 : 来源: 样品 :复方丹参片 批号 : 来源: 试剂名称:乙腈 批号 : 来源: 来源: 试剂名称:甲醇 批号 : 空白对照物:按复方丹参片质量标准制法自制(缺三七) 8.2.2. 仪器: 高效液相色谱仪型号: 编号: 色谱柱编号: 分析天平型号 : 编号: 超声处理器型号: 编号: rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 8.2.3(溶液配置: 8.2.3.1.对照品溶液配置 精密称取人参皂苷Rg对照品、人参皂苷Rb对照11品、人参皂苷R对照品、人参皂苷Re对照品适量,加70%甲醇制成每1ml含参1 皂苷Rg及人参皂苷Rb各0.2mg、人参皂苷R及人参皂苷Re各0.05mg的混合111 溶液即得。 8.2.3.2供试品溶液 取复方丹参片10片,除去糖衣片,精密称定,研细, 取约1g,精密称定后置50ml具塞量瓶中,加70%甲醇50ml并称定重量,超声处理30分钟,放冷,称定重量,用70%甲醇补足减失的重量,摇匀滤过,取续滤液即得。 8.2.3.3. 空白物溶液 取空白物10片,除去糖衣片,精密称定,研细, 取约1g,精密称定后置50ml具塞量瓶中,加70%甲醇50ml并称定重量,超声处理30分钟,放冷,称定重量,用70%甲醇补足减失的重量,摇匀滤过,取续滤液即得。 8.2.4 分析方法: 用十八烷基硅烷键合硅胶为填充剂用十八烷基硅烷键合硅胶为填充剂;以乙腈为流动项A,以水为流动项B,按表1的规定进行梯度洗脱,进样量为20 ul。 8.3.检验方法的确认 8.3.1专属性 8.3.1.1 色谱条件与系统适用性试验 用十八烷基硅烷键合硅胶为填充剂;以乙腈为流动相A,以水为流动相B,按表2的规定进行梯度洗脱检测波长为203nm。理论板数以人参皂苷Rg峰计算应不低于6000,人参皂苷Rg与人参皂11苷Re的分离度应大于1.8. 8.3.1.2. 测定 分别精密吸取对照品溶液与空白样品溶液各20µl,注入液相色谱仪,测定,记录色谱图。 8.3.1.3. 确认合格标准 空白样品溶液在与对照品溶液相同的保留间 处色谱峰峰面积小于对照品峰面积的3%。 8.3.2.精密度 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities 8.3.2.1重复性 8.3.2.1.1. 取同一浓度的对照品溶液及供试品溶液分别连续进样6针,记录色谱图。 8.3.2.1.2. 确认合格标准 6针对照品溶液、供试品溶液峰面积的RSD应不得超过2.0%。 8.3.2.2中间精密度 8.3.2.2.1. 在不同的日期和不同的仪器,不同检验员(3人)按8.2.3.2的方法重新制备样液,分别计算含量。 8.3.2.2.2. 确认合格标准 每人RSD应不得超过2.0%,3人RSD应不得超过2.0%。 8.3.3准确度 8.3.3.1精密称取人参皂苷Rg对照品、人参皂苷Rb对照品、人参皂苷R对111照品、人参皂苷Re对照品适量,加70%甲醇制成每1ml含参皂苷Rg及人参皂1苷Rb各0.2mg、人参皂苷R及人参皂苷Re各0.05mg的对照品溶液。 11 取上述(8.2.3.2)研细的复方丹参片样品0.6g,精密称定10份,分别置于具塞量瓶中,并分别加入对照品溶液0、10、10、10、20、20、20、30、30、30ml,超声处理30分钟,放冷后用70%甲醇补足至刻度,摇匀离心取上清夜即得。 8.3.3.2精密吸取10份样液各20ul,注入液相色谱仪,测定,计算回收率。 计算公式: 测得值-样品中的量 ×100% 回收率(%)= 加入的对照品量 8.3.3.3(确认合格标准 人参皂苷Rg、人参皂苷Rb、人参皂苷R、人参皂111苷Re的加样回收率收率98.0%,102%,回收率的RSD小于2.0%。 rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities rAt present, we have formed a "three-three" Park. …… Industrial Park, according to ... ... The instructions of comrade, focus on development needs in the next decade, based on the original, and then extended the 6 square kilometers. Of the Park, to further improve the roads, power supply, communications, water supply and drainage and sewage pipe network and other infrastructure, to achieve full coverage of infrastructure and interconnection with the facilities and raise capacity. Each park to determine 1 leading industries, in particular stone Materials, cans, gloves, through guided, force and other measures to promote the "road company" Park, industrial agglomeration. Currently, to focus on building better ... ... Industrial Park, ... ... Wood Park as the starting area of the industrial park, planners need to take out plan, start construction as soon as possible, undertake in a timely manner ... ... Transfer of the wood industry. This opportunity slip by, so the timing must be tight. Second is to optimize government service. Low efficiency of government services, departments do not coordinate the views of businesses large, poor business environment, it is ... ... Short Board, decide to change. We will continue to deepen reform of the administrative examination and approval system, good digestion, implement the Government canceled, adjustment and devolution of administrative examination and approval matters, strengthen the existing supervision in matters of administrative power, has made it clear to cancel, are not allowed to keep or disguised approval. To do list list of administrative powers and responsibilities
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