HH-624毛细管柱 中国药典2015 二部 乙醇量测定

固定液：6%氰丙基苯基-94%甲基聚硅氧烷

极性： 中等极性

使用温度：40℃～240℃

规格：30m*0.53mm*3um

型号：HH-624

应用：中国药典2015 二部 乙醇量测定

法（毛细管柱法）
色谱条件与系统适用性试验  采用（6%）氰丙基苯基-（94%）二甲基聚硅氧烷为固定液的毛细管柱；起始温度为40℃，维持2分钟，以每分钟3℃的速率升温65℃，再以每分钟25℃的速率升温200℃，维持10分钟；进样口温度200℃；检测器（FID）温度220℃；采用顶空分流进样，分流比为1：1；顶空瓶平衡温度为85℃，平衡时间为20分钟。理论板数按乙醇峰计算应不低于10000，乙醇峰与正丙醇峰的分离度应大于2.0。
校正因子测定 精密量取恒温20℃的无水乙醇5ml，平行两份；置100ml量瓶中，精密加入恒温20℃的正丙醇（内标物质）5ml，用水稀释刻度，摇匀，精密量取该溶液1ml，置100ml量瓶中，用水稀释刻度，摇匀（必要时可进一步稀释），作为对照品溶液。精密量取3ml，置10ml顶空进样瓶中，密封，顶空进样，每份对照品溶液进样3次，测定峰面积，计算平均校正因子，所得校正因子的相对标准偏差不得大于2.0%。
测定法 精密量取恒温20℃的供试品适量（相当于乙醇约5ml），置100ml量瓶中，精密加入恒温20℃的正丙醇5ml，用水稀释刻度，摇匀，精密量取该溶液1ml，置100ml量瓶中，用水稀释刻度，摇匀（必要时可进一步稀释），作为供试品溶液。精密量取3ml，置10ml顶空进样瓶中，密封，顶空进样，测定峰面积，按内标法以峰面积计算，即得。
【附注】毛细管柱建议选择大口径、厚液膜色谱柱，规格为30m×0.53mm×3.00μm。


中国药典2015 二部 乙醇量测定 测试谱图：


Chinese Pharmacopoeia 2015 Part Two Determination of Ethanol Amount
Chinese Pharmacopoeia 2015 Part Two Detailed information on determination of ethanol content:


Name: Capillary Column
Fixing fluid: 6% cyanopropyl phenyl-94% methyl polysiloxane

Polarity: medium polarity

Operating temperature: 40℃～240℃

Specification: 30m*0.53mm*3um

Model: HH-624

Application: 2015 Chinese Pharmacopoeia Part II Determination of ethanol content

The first method (capillary column method)
The chromatographic conditions and system suitability test use (6%) cyanopropyl phenyl-(94%) dimethyl polysiloxane as the fixed liquid capillary column; the starting temperature is 40 ℃, maintained for 2 minutes, every minute The temperature is increased to 65°C at a rate of 3°C, and then to 200°C at a rate of 25°C per minute, and maintained for 10 minutes; the temperature of the injection port is 200°C; the temperature of the detector (FID) is 220°C; headspace split sampling is used, split flow The ratio is 1:1; the equilibrium temperature of the headspace bottle is 85℃, and the equilibrium time is 20 minutes. The number of theoretical plates should not be less than 10,000 calculated based on the ethanol peak, and the separation between the ethanol peak and the n-propanol peak should be greater than 2.0.
Correction factor determination. Precisely measure 5ml of absolute ethanol at a constant temperature of 20°C, in parallel; place in a 100ml measuring flask, precisely add 5ml of n-propanol (internal standard substance) at a constant temperature of 20°C, dilute to the mark with water, and shake well , Accurately measure 1ml of the solution, put it in a 100ml measuring flask, dilute to the mark with water, shake it up (if necessary, further dilute), as a reference solution. Accurately measure 3ml, place it in a 10ml headspace sampling bottle, seal, and inject headspace, each reference solution is injected 3 times, the peak area is measured, and the average correction factor is calculated. The relative standard deviation of the obtained correction factor shall not be greater than 2.0 %.
Assay method Precisely measure an appropriate amount of the test product (equivalent to about 5ml of ethanol) at a constant temperature of 20°C, place it in a 100ml measuring flask, and add 5ml of n-propanol at a constant temperature of 20°C, dilute to the mark with water, shake well, and measure accurately Take 1ml of the solution, put it in a 100ml measuring flask, dilute to the mark with water, shake it up (if necessary, further dilute), as the test solution. Accurately measure 3ml, place it in a 10ml headspace sample bottle, seal it, inject the sample in the headspace, measure the peak area, and calculate the peak area according to the internal standard method.
[Note] The capillary column is recommended to choose a large-diameter, thick liquid film chromatography column, the specification is 30m×0.53mm×3.00μm.


Chinese Pharmacopoeia 2015 Part Two Determination of the amount of ethanol Test spectrum: