CN107957477B - A kind of method that adopts non-aqueous titration method to measure posaconazole content - Google Patents
A kind of method that adopts non-aqueous titration method to measure posaconazole content Download PDFInfo
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- RAGOYPUPXAKGKH-XAKZXMRKSA-N posaconazole Chemical compound O=C1N([C@H]([C@H](C)O)CC)N=CN1C1=CC=C(N2CCN(CC2)C=2C=CC(OC[C@H]3C[C@@](CN4N=CN=C4)(OC3)C=3C(=CC(F)=CC=3)F)=CC=2)C=C1 RAGOYPUPXAKGKH-XAKZXMRKSA-N 0.000 title claims abstract description 75
- 229960001589 posaconazole Drugs 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004448 titration Methods 0.000 title claims abstract description 29
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims abstract description 107
- 239000012086 standard solution Substances 0.000 claims abstract description 51
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 36
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229960000583 acetic acid Drugs 0.000 claims abstract description 18
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 18
- 238000003918 potentiometric titration Methods 0.000 claims abstract description 18
- 239000012046 mixed solvent Substances 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000004458 analytical method Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 11
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 208000009329 Graft vs Host Disease Diseases 0.000 description 1
- 206010061598 Immunodeficiency Diseases 0.000 description 1
- 208000037026 Invasive Fungal Infections Diseases 0.000 description 1
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- 238000002512 chemotherapy Methods 0.000 description 1
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- 208000024908 graft versus host disease Diseases 0.000 description 1
- 210000003958 hematopoietic stem cell Anatomy 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 208000032839 leukemia Diseases 0.000 description 1
- 201000002364 leukopenia Diseases 0.000 description 1
- 231100001022 leukopenia Toxicity 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000011321 prophylaxis Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明属于分析化学领域，具体涉及一种采用非水滴定法测定泊沙康唑含量的方法。The invention belongs to the field of analytical chemistry, and in particular relates to a method for determining the content of posaconazole by using a non-aqueous titration method.
背景技术Background technique
泊沙康唑(posaconazole)化学名为4-[4-[4-[4-[[(3R,5R)-5-(2,4-二氟苯基)-5-(1,2,4-三唑-1-基甲基)氧杂戊环-3-基]甲氧基]苯基]哌嗪-1-基]苯基]-2-[(2S,3S)-2-羟基戊-3-基]-1,2,4-三唑-3-酮。泊沙康唑的结构式如下：Posaconazole (posaconazole) chemical name is 4-[4-[4-[4-[[(3R,5R)-5-(2,4-difluorophenyl)-5-(1,2,4 -Triazol-1-ylmethyl)oxolane-3-yl]methoxy]phenyl]piperazin-1-yl]phenyl]-2-[(2S,3S)-2-hydroxypentan -3-yl]-1,2,4-triazol-3-one. The structural formula of posaconazole is as follows:
泊沙康唑适用于多种对两性霉素不能耐受或难治性成人侵袭性真菌感染的治疗，可对高危患者进行预防用药，如用于13岁以上、免疫功能低下的患者，特别是患有移植物抗宿主病的造血干细胞移植者、白血病患者和由于化疗而长期白细胞减少的患者。因此，泊沙康唑在临床上被广泛的应用。Posaconazole is suitable for the treatment of a variety of amphotericin-intolerant or refractory adult invasive fungal infections, and can be used for prophylaxis in high-risk patients, such as those over 13 years old and immunocompromised, especially Hematopoietic stem cell transplant recipients with graft-versus-host disease, leukemia patients, and patients with chronic leukopenia due to chemotherapy. Therefore, posaconazole is widely used in clinical practice.
目前，对泊沙康唑含量的检测方法少有报道，仅有高效液相色谱法测定其含量；与色谱法相比较，容量法的准确度更高。因此，研制开发一种采用非水滴定法测定泊沙康唑含量的方法一直是亟待解决的新课题。At present, there are few reports on the detection method of posaconazole content, and only high performance liquid chromatography is used to determine its content; compared with chromatography, the volumetric method has higher accuracy. Therefore, research and development of a non-aqueous titration method for the determination of posaconazole content has always been a new subject to be solved.
发明内容SUMMARY OF THE INVENTION
基于现有技术的不足，本发明的目的在于提供一种采用非水滴定法测定泊沙康唑含量的方法，该方法所使用的仪器设备简单、原料易得、成本低、操作简便、省时节料。Based on the deficiencies of the prior art, the object of the present invention is to provide a method for measuring the content of posaconazole by using a non-aqueous titration method. .
为了实现上述目的，本发明采用的技术方案为：In order to achieve the above object, the technical scheme adopted in the present invention is:
一种采用非水滴定法测定泊沙康唑含量的方法，以丁酮和冰醋酸组成的混合溶剂，定量溶解泊沙康唑，用高氯酸标准溶液为滴定剂，采用电位滴定法进行滴定；A method for determining the content of posaconazole by using a non-aqueous titration method, using a mixed solvent composed of butanone and glacial acetic acid to quantitatively dissolve the posaconazole, using a standard solution of perchloric acid as a titrant, and using a potentiometric titration method for titration;
泊沙康唑含量＝[(V-V0)×C×0.03504/(0.1×M)]×100%；Content of posaconazole=[(VV 0 )×C×0.03504/(0.1×M)]×100%;
其中：V—泊沙康唑消耗高氯酸标准溶液的体积，单位为mL；V0—空白消耗高氯酸标准溶液的体积，单位为mL；C—高氯酸标准溶液浓度，单位为mol/L；M—泊沙康唑重量，单位为g。Wherein: V—posaconazole consumes the volume of perchloric acid standard solution, the unit is mL; V 0 —blank consumes the volume of perchloric acid standard solution, the unit is mL; C—perchloric acid standard solution concentration, the unit is mol /L; M—weight of posaconazole, in g.
优选地，组成混合溶剂的丁酮和冰醋酸的体积比为4~6:1。Preferably, the volume ratio of butanone and glacial acetic acid constituting the mixed solvent is 4 to 6:1.
进一步，组成混合溶剂的丁酮和冰醋酸的体积比为5:1。Further, the volume ratio of butanone and glacial acetic acid constituting the mixed solvent is 5:1.
优选地，定量溶解泊沙康唑时，泊沙康唑的质量与混合溶剂的体积之比为1:100~115 g/mL。Preferably, when quantitatively dissolving posaconazole, the ratio of the mass of posaconazole to the volume of the mixed solvent is 1:100-115 g/mL.
进一步，定量溶解泊沙康唑时，泊沙康唑的质量与混合溶剂的体积之比为1:107g/mL。Further, when posaconazole was quantitatively dissolved, the ratio of the mass of posaconazole to the volume of the mixed solvent was 1:107 g/mL.
优选地，所述高氯酸标准溶液的溶剂是无水冰醋酸。Preferably, the solvent of the perchloric acid standard solution is anhydrous glacial acetic acid.
优选地，所述高氯酸标准溶液的浓度为0.08~0.12 mol/L。Preferably, the concentration of the perchloric acid standard solution is 0.08-0.12 mol/L.
进一步，所述高氯酸标准溶液的浓度为0.1 mol/L。Further, the concentration of the perchloric acid standard solution is 0.1 mol/L.
优选地，所述的电位滴定法是指用通过测量电位变化确定终点并计算泊沙康唑含量。Preferably, the potentiometric titration method refers to determining the end point by measuring the potential change and calculating the posaconazole content.
本发明鉴于泊沙康唑可以与高氯酸发生反应，从而采用非水滴定法测定泊沙康唑含量。与现有技术相比，本发明具有仪器设备简单、操作简便、成本低、易于掌握、精密度高、含量准确、重复性好等优点，将广泛地应用于化学分析领域中。In view of the fact that posaconazole can react with perchloric acid, the present invention adopts a non-aqueous titration method to measure the content of posaconazole. Compared with the prior art, the invention has the advantages of simple equipment, simple operation, low cost, easy to grasp, high precision, accurate content, good repeatability, etc., and will be widely used in the field of chemical analysis.
附图说明Description of drawings
图1是实施例1泊沙康唑的电极电位对体积的曲线图；Fig. 1 is the graph of the electrode potential of embodiment 1 posaconazole to volume;
图2是实施例1泊沙康唑的电极电位对体积的一阶导数曲线图；Fig. 2 is the first derivative curve diagram of the electrode potential of embodiment 1 posaconazole to volume;
图3是实施例1泊沙康唑的电极电位对体积的二阶导数曲线图。3 is a graph of the second derivative curve of electrode potential versus volume of posaconazole in Example 1. FIG.
具体实施方式Detailed ways
为了使本发明的技术目的、技术方案和有益效果更加清楚，下面结合具体实施例对本发明的技术方案作出进一步的说明，但所述实施例旨在解释本发明，而不能理解为对本发明的限制，实施例中未注明具体技术或条件者，按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。In order to make the technical purpose, technical solution and beneficial effect of the present invention clearer, the technical solution of the present invention will be further described below in conjunction with specific embodiments, but the embodiments are intended to explain the present invention and should not be construed as limiting the present invention , if no specific technology or conditions are indicated in the examples, the technology or conditions described in the literature in the field or the product specification are used.
实施例1Example 1
一种采用非水滴定法测定泊沙康唑含量的方法，以丁酮和冰醋酸组成的混合溶剂，定量溶解泊沙康唑，用高氯酸标准溶液为滴定剂，采用电位滴定法进行滴定。A method for determining the content of posaconazole by using a non-aqueous titration method. The mixed solvent composed of butanone and glacial acetic acid is used to quantitatively dissolve posaconazole, and a standard solution of perchloric acid is used as a titrant, and the potentiometric titration method is used for titration.
其中，高氯酸标准溶液的浓度为0.1 mol/L，其配制方法为：取无水冰醋酸（按含水量计算，每1g水加醋酐5.22 mL）750 mL，加高氯酸（70%~72%）8.5 mL，摇匀，在室温下缓缓滴加醋酐23 mL，边加边摇，加完后再振摇均匀，放冷，加无水冰醋酸使成1000 mL，摇匀，放置24小时。Among them, the concentration of perchloric acid standard solution is 0.1 mol/L, and its preparation method is as follows: take 750 mL of anhydrous glacial acetic acid (calculated by water content, add 5.22 mL of acetic anhydride per 1 g of water), add perchloric acid (70% ~72%) 8.5 mL, shake well, slowly add 23 mL of acetic anhydride dropwise at room temperature, shake while adding, shake well after adding, let cool, add anhydrous glacial acetic acid to make 1000 mL, shake well , left for 24 hours.
0.1 mol/L高氯酸标准溶液的标定：取在105℃干燥至恒重的基准邻苯二甲酸氢钾0.16 g，精密称定，加无水冰醋酸20 mL使其溶解，摇匀，按照电位滴定法，用待标定的高氯酸标准溶液进行滴定，用电位滴定指示终点，并将滴定结果用空白试验进行校正。每1 mL高氯酸标准溶液（0.1 ml/L）相当于20.42 mg的邻苯二甲酸氢钾，根据待标定的高氯酸标准溶液消耗量与邻苯二甲酸氢钾的取用量，算出待标定的高氯酸标准溶液的浓度，即得。Calibration of 0.1 mol/L perchloric acid standard solution: Take 0.16 g of benchmark potassium hydrogen phthalate dried to constant weight at 105 °C, accurately weigh, add 20 mL of anhydrous glacial acetic acid to dissolve, shake well, and follow Potentiometric titration method, titrate with perchloric acid standard solution to be calibrated, use potentiometric titration to indicate the end point, and correct the titration result with blank test. Each 1 mL perchloric acid standard solution (0.1 ml/L) is equivalent to 20.42 mg of potassium hydrogen phthalate. According to the consumption of perchloric acid standard solution to be calibrated and the amount of potassium hydrogen phthalate to be calibrated, calculate The concentration of the calibrated perchloric acid standard solution is obtained.
高氯酸标准溶液浓度C(mol/L)=m×0.1×1000/(V样-V空)×20.42Concentration of perchloric acid standard solution C(mol/L)=m×0.1×1000/(V sample- V empty )×20.42
其中C为高氯酸标准溶液浓度，mol/L；Wherein C is the concentration of perchloric acid standard solution, mol/L;
m为基准邻苯二甲酸氢钾的称取量，mg；m is the weighing amount of the benchmark potassium hydrogen phthalate, mg;
V样为标定中高氯酸标准溶液的用量，mL；V sample is the amount of standard solution of perchloric acid in the calibration, mL;
V空为空白试验中高氯酸标准溶液的用量，mL。V is the amount of perchloric acid standard solution in the blank test, mL.
由于冰醋酸的膨胀系数较大，所以若滴定样品和标定高氯酸标准溶液时的温度差别超过10℃时，重新进行标定，若未超过10℃时，应对温度引起体积的改变进行校正，校正公式如下：Due to the large expansion coefficient of glacial acetic acid, if the temperature difference between the titrated sample and the perchloric acid standard solution exceeds 10°C, re-calibrate. If it does not exceed 10°C, the volume change caused by temperature should be corrected. The formula is as follows:
C1=C0/(1+0.0011×(t1- t0))C 1 =C 0 /(1+0.0011×(t 1 - t 0 ))
其中，0.0011为冰醋酸的膨胀系数；Wherein, 0.0011 is the expansion coefficient of glacial acetic acid;
t0为标定高氯酸标准溶液的温度；t 0 is the temperature of calibrating perchloric acid standard solution;
t1为滴定泊沙康唑时的温度；t 1 is the temperature when titrating posaconazole;
C0为t0时高氯酸标准溶液的浓度；C 0 is the concentration of perchloric acid standard solution at t 0 ;
C1为t1时高氯酸标准溶液的浓度。C 1 is the concentration of perchloric acid standard solution at t 1 .
测定方法：精密称取泊沙康唑样品0.56 g，加混合溶剂（丁酮和冰醋酸的体积比为5:1）60 mL，摇匀，按照电位滴定法，用0.1 mol/L高氯酸标准溶液进行滴定，用电位滴定指示终点，并将滴定结果用空白试验进行校正。每1 mL的0.1mol/L高氯酸标准溶液相当于35.04 mg泊沙康唑。Determination method: Precisely weigh 0.56 g of posaconazole sample, add 60 mL of mixed solvent (the volume ratio of butanone and glacial acetic acid is 5:1), shake well, and use 0.1 mol/L perchloric acid according to the potentiometric titration method. The standard solution is titrated, the end point is indicated by potentiometric titration, and the titration result is corrected by blank test. Each 1 mL of 0.1 mol/L perchloric acid standard solution is equivalent to 35.04 mg of posaconazole.
计算公式：泊沙康唑含量（%）=[(V-V0)×C×0.03504/(0.1×M)]×100%Calculation formula: posaconazole content (%)=[(VV 0 )×C×0.03504/(0.1×M)]×100%
其中：V—泊沙康唑消耗高氯酸标准溶液的体积，单位为mL；Wherein: V—the volume of perchloric acid standard solution consumed by posaconazole, the unit is mL;
V0—空白消耗高氯酸标准溶液的体积，单位为mL；V 0 —the volume of the standard solution of perchloric acid consumed by the blank, in mL;
C—高氯酸标准溶液浓度，单位为mol/L；C—concentration of perchloric acid standard solution, the unit is mol/L;
M—泊沙康唑重量，单位为g。M—weight of posaconazole, in g.
注：每1 mL 0.1 mol/L高氯酸标准溶液相当于35.04 mg泊沙康唑。Note: Each 1 mL of 0.1 mol/L perchloric acid standard solution is equivalent to 35.04 mg of posaconazole.
实际测定：精密称重泊沙康唑样品0 .56055g，用0 .09984mol/L(t0＝23 .2℃)高氯酸标准溶液滴定，用电位滴定指示终点，并将滴定结果用空白试验进行校正，空白消耗高氯酸标准溶液0 .02mL。参见图1、图2和图3，从图3中可以看出电极电位对体积的二阶导数与X轴交点为15 .766mL，即为滴定终点。滴定泊沙康唑时的温度t1＝25℃，校正后高氯酸标准溶液的浓度计算泊沙康唑含量(%)＝99 .88%。Actual determination: Precisely weigh 0.56055g posaconazole sample, titrate with 0.09984mol/L (t0=23.2℃) perchloric acid standard solution, use potentiometric titration to indicate the end point, and use the blank test for the titration result For calibration, the blank consumes 0.02 mL of perchloric acid standard solution. Referring to Figure 1, Figure 2 and Figure 3, it can be seen from Figure 3 that the intersection of the second derivative of the electrode potential to the volume and the X axis is 15.766mL, which is the end point of the titration. The temperature t1=25℃ when titrating posaconazole, the concentration of perchloric acid standard solution after correction calculates the content of posaconazole (%)=99.88%.
重复性试验：精密称取泊沙康唑，按照电位滴定法连续测定6次，空白消耗高氯酸标准溶液为0.020 mL，测定结果为99.76%，相对偏差为0.03%，试验结果表明，本方法重复性好，完全符合含量测定的质量控制要求，泊沙康唑含量测定精密度实验结果见表1。Repeatability test: Precisely weigh posaconazole and measure it continuously for 6 times according to the potentiometric titration method. The blank consumption of perchloric acid standard solution is 0.020 mL, the measurement result is 99.76%, and the relative deviation is 0.03%. The test results show that this method The repeatability is good, and it fully meets the quality control requirements of content determination. The experimental results of the precision of posaconazole content determination are shown in Table 1.
表1 泊沙康唑含量测定精密度试验结果Table 1 The results of the precision test for the determination of posaconazole
对比例1Comparative Example 1
一种采用非水滴定法测定泊沙康唑含量的方法，以冰醋酸为溶剂，定量溶解泊沙康唑，用高氯酸标准溶液为滴定剂，采用电位滴定法进行滴定。A non-aqueous titration method is used to determine the content of posaconazole. Glacial acetic acid is used as a solvent to quantitatively dissolve posaconazole, and a standard solution of perchloric acid is used as a titrant, and potentiometric titration is used for titration.
其中，高氯酸标准溶液的浓度为0.1 mol/L，其配制方法同实施例1。Wherein, the concentration of perchloric acid standard solution is 0.1 mol/L, and its preparation method is the same as that of Example 1.
0.1 mol/L高氯酸标准溶液的标定同实施例1。The calibration of the 0.1 mol/L perchloric acid standard solution is the same as that in Example 1.
测定方法：精密称取泊沙康唑样品0.56 g，加冰醋酸60ml，摇匀，按照电位滴定法，用0.1 mol/L高氯酸标准溶液进行滴定，用电位滴定指示终点，并将滴定结果用空白试验进行校正。每1 mL的0.1mol/L高氯酸标准溶液相当于35.04 mg泊沙康唑。Determination method: Precisely weigh 0.56 g of posaconazole sample, add 60 ml of glacial acetic acid, shake well, titrate with 0.1 mol/L perchloric acid standard solution according to potentiometric titration method, use potentiometric titration to indicate the end point, and titrate the titration method. The results were corrected with a blank test. Each 1 mL of 0.1 mol/L perchloric acid standard solution is equivalent to 35.04 mg of posaconazole.
计算公式：泊沙康唑含量（%）=[(V-V0)×C×0.03504/(0.1×M)]×100%Calculation formula: posaconazole content (%)=[(VV 0 )×C×0.03504/(0.1×M)]×100%
其中：V—泊沙康唑消耗高氯酸标准溶液的体积，单位为mL；Wherein: V—the volume of perchloric acid standard solution consumed by posaconazole, the unit is mL;
V0—空白消耗高氯酸标准溶液的体积，单位为mL；V 0 —the volume of the standard solution of perchloric acid consumed by the blank, in mL;
C—高氯酸标准溶液浓度，单位为mol/L；C—concentration of perchloric acid standard solution, the unit is mol/L;
M—泊沙康唑重量，单位为g。M—weight of posaconazole, in g.
注：每1 mL 0.1 mol/L高氯酸标准溶液相当于35.04 mg泊沙康唑。Note: Each 1 mL of 0.1 mol/L perchloric acid standard solution is equivalent to 35.04 mg of posaconazole.
实际测定：精密称重泊沙康唑样品0.56055g，测定消耗0.09984mol/L（t0=23.2℃）高氯酸标准溶液的体积，用电位滴定指示终点，并将滴定结果用空白试验进行校正，空白消耗高氯酸标准溶液0.02 mL。滴定结果显示没有明显到突跃，电极电位对体积的二阶导数与X轴交点9个，无法确定终点，也无法计算泊沙康唑含量。Actual determination: Precisely weigh 0.56055g of posaconazole sample, measure the volume of perchloric acid standard solution that consumes 0.09984mol/L (t 0 =23.2°C), use potentiometric titration to indicate the end point, and carry out the titration result with a blank test For calibration, the blank consumes 0.02 mL of perchloric acid standard solution. The titration results showed that there was no obvious sudden jump, and there were 9 intersections between the second derivative of the electrode potential to the volume and the X-axis. The end point could not be determined, and the content of posaconazole could not be calculated.
重复性试验：精密称取泊沙康唑，按照电位滴定法连续测定6次，均无法找到突跃点，不能计算泊沙康唑到含量。试验结果表明，对比例1无法计算含量，不符合含量测定的质量控制要求。Repeatability test: Posaconazole was accurately weighed, and measured continuously for 6 times according to the potentiometric titration method, but the sudden jump point could not be found, and the content of posaconazole could not be calculated. The test results show that the content of Comparative Example 1 cannot be calculated, and it does not meet the quality control requirements for content determination.
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