Method for Removing Organic Solvent from Starch Hemostatic Microspheres

Abstract

The present invention provides a method for removing an organic solvent from starch hemostatic microspheres, comprising the following steps: 1. taking to-be-dried starch hemostatic microspheres and laying them flatly on drying trays with attention to laying them as uniformly and thinly as possible; 2. taking an adsorbent and subpackaging it into dialyzing paper bags for sealing; and 3. placing the trays and the dialyzing paper bags completed in the previous two steps on separators of a low-temperature vacuum oven in layers, setting the oven temperature at 0-20° C., then vacuumizing and keeping pressure for 15-48 hours. The method provided by the present invention can reduce organic solvent residue in the starch hemostatic microspheres to less than 0.05%, which meets the requirements of relevant standards for medical devices, thereby improving safety of products.

Claims

1. A method for removing an organic solvent from starch hemostatic microspheres, comprising the following steps: (1) taking to-be-dried starch hemostatic microspheres and laying them flatly on drying trays; (2) taking an adsorbent according to a mass ratio of 20%˜100% of a to-be-dried product and subpackaging it into dialyzing paper bags for sealing, wherein the adsorbent is an adsorbent capable of adsorbing organic gases; and (3) placing the trays loaded with the starch hemostatic microspheres and the dialyzing paper bags loaded with the adsorbent on separators of a low-temperature vacuum oven in layers, setting the oven temperature at 0-20° C., then vacuumizing to a negative pressure of −0.1˜−0.05 MPa, and keeping pressure for 15˜48 hours.

2. The method for removing the organic solvent from the starch hemostatic microspheres according to claim 1, wherein the adsorbent is a solid being one or more selected from activated carbon, molecular sieve, clay, metal-organic frameworks (MOFs) and polymeric adsorbent resin and having an ability to dry the organic gases and a physical absorption function.

Description

BRIEF DESCRIPTION OF DRAWINGS

[0017] FIG. 1 is a schematic diagram of embodiments of the present invention; in FIG. 1: 1. Low-temperature vacuum oven, 2. Oven body, 3. Separators, 4. Trays placed in layers for to-be-dried samples, and 5. Dialyzing paper bags placed in layers and loaded with adsorbents.

[0018] FIG. 2 shows GC testing results of residual ethyl alcohol and ethyl acetate in starch hemostatic microspheres treated by Embodiment 1 of the present invention.

DETAILED DESCRIPTION

[0019] The substantive features and notable progress of the present invention are further clarified by introducing embodiments of the present invention, but the present invention is by no means limited to the embodiments.

Embodiment 1

[0020] (1) To-be-dried starch hemostatic microspheres were taken and laid flatly on drying trays with attention to laying them as uniformly and thinly as possible;

[0021] (2) activated carbon particles were taken according to a mass ratio of 55% of a to-be-dried product and subpackaged into dialyzing paper bags to be sealed; and

[0022] (3) as shown in FIG. 1, the trays loaded with the starch hemostatic microspheres and the dialyzing paper bags loaded with an adsorbent were placed on separators 3 in an oven body 2 of a low-temperature vacuum oven 1 in layers, after placing, the positions were as shown in 4 and 5, an oven door was closed, the temperature of the oven 1 was set at 12° C., then vacuumizing was conducted to −0.08 MPa, and the pressure was kept for 24 hours.

[0023] After the product was taken to be subjected to enzymolysis with amylase in purified water, the content of ethyl alcohol and ethyl acetate in the starch hemostatic microspheres was tested through a GC method, as shown in FIG. 2, wherein data were shown in the following table.

TABLE-US-00002 Sample 0.5018 g starch hemostatic microspheres preparation in 5.0 mL purified water Ret. time of 3.733 Ret. time of 6.449 ethyl alcohol ethyl acetate Area of ethyl 9226 Area of ethyl 3994 alcohol acetate Content of 0.030% Content of 0.020% ethyl alcohol ethyl acetate

Embodiment 2

[0024] (1) An appropriate number of to-be-dried starch hemostatic microspheres were taken and laid flatly on drying trays with attention to laying them as uniformly and thinly as possible;

[0025] (2) a 4A molecular sieve was taken according to a mass ratio of 60% of a to-be-dried product and subpackaged into dialyzing paper bags to be sealed; and

[0026] (3) as shown in FIG. 1, the trays loaded with the starch hemostatic microspheres and the dialyzing paper bags loaded with an adsorbent were placed on separators 3 in an oven body 2 of a low-temperature vacuum oven 1 in layers, after placing, the positions were as shown in 4 and 5, an oven door was closed, the temperature of the oven 1 was set at 20° C., then vacuumizing was conducted to −0.05 MPa, and the pressure was kept for 15 hours.

[0027] After the product was taken to be subjected to enzymolysis with amylase in purified water, the content of ethyl alcohol and ethyl acetate in the starch hemostatic microspheres was tested through a GC method, as shown in the following table.

TABLE-US-00003 Content of ethyl alcohol 0.008% Content of ethyl acetate 0.009%

Embodiment 3

[0028] (1) An appropriate number of to-be-dried starch hemostatic microspheres were taken and laid flatly on drying trays with attention to laying them as uniformly and thinly as possible;

[0029] (2) clay was taken according to a mass ratio of 100% of a to-be-dried product and subpackaged into dialyzing paper bags to be sealed; and

[0030] (3) as shown in FIG. 1, the trays loaded with the starch hemostatic microspheres and the dialyzing paper bags loaded with an adsorbent were placed on separators 3 in an oven body 2 of a low-temperature vacuum oven 1 in layers, after placing, the positions were as shown in 4 and 5, an oven door was closed, the temperature of the oven was set at 0° C., then vacuumizing was conducted to −0.1 MPa, and the pressure was kept for 48 hours.

[0031] After the product was taken to be subjected to enzymolysis with amylase in purified water, the content of ethyl alcohol and ethyl acetate in the starch hemostatic microspheres was tested through a GC method, as shown in the following table.

TABLE-US-00004 Content of ethyl alcohol 0.006% Content of ethyl acetate 0.010%

Embodiment 4

[0032] (1) An appropriate number of to-be-dried starch hemostatic microspheres were taken and laid flatly on drying trays with attention to laying them as uniformly and thinly as possible;

[0033] (2) metal-organic frameworks (MOFs) were taken according to a mass ratio of 20% of a to-be-dried product and subpackaged into dialyzing paper bags to be sealed; and

[0034] (3) as shown in FIG. 1, the trays loaded with the starch hemostatic microspheres and the dialyzing paper bags loaded with an adsorbent were placed on separators 3 in an oven body 2 of a low-temperature vacuum oven 1 in layers, after placing, the positions were as shown in 4 and 5, an oven door was closed, the temperature of the oven was set at 0° C., then vacuumizing was conducted to −0.1 MPa, and the pressure was kept for 48 hours.

[0035] After the product was taken to be subjected to enzymolysis with amylase in purified water, the content of ethyl alcohol and ethyl acetate in the starch hemostatic microspheres was tested through a GC method, as shown below.

TABLE-US-00005 Content of ethyl alcohol 0.020% Content of ethyl acetate 0.008%

Embodiment 5

[0036] (1) An appropriate number of to-be-dried starch hemostatic microspheres were taken and laid flatly on drying trays with attention to laying them as uniformly and thinly as possible;

[0037] (2) polymeric adsorbent resin was taken according to a mass ratio of 50% of a to-be-dried product and subpackaged into dialyzing paper bags to be sealed; and

[0038] (3) as shown in FIG. 1, the trays loaded with the starch hemostatic microspheres and the dialyzing paper bags loaded with an adsorbent were placed on separators 3 in an oven body 2 of a low-temperature vacuum oven 1 in layers, after placing, the positions were as shown in 4 and 5 an oven door was closed, the temperature of the oven was set at 0° C., then vacuumizing was conducted to −0.1 MPa, and the pressure was kept for 48 hours.

[0039] After the product was taken to be subjected to enzymolysis with amylase in purified water, the content of ethyl alcohol and ethyl acetate in the starch hemostatic microspheres was tested through a GC method, as shown below.

TABLE-US-00006 Content of ethyl alcohol 0.023% Content of ethyl acetate 0.008%

Embodiment 6

[0040] (1) Starch hemostatic microspheres were taken according to the method of Embodiment 1 to be dried, and this batch was marked as NO.1;

[0041] (2) the same number of to-be-dried starch hemostatic microspheres were taken and uniformly and thinly laid on drying trays flatly, and this batch was marked as NO.2; and

[0042] (3) the trays loaded with sample NO.2 were placed in a common vacuum oven, the oven temperature was set at 70° C., a vacuum was set to be −0.1MPa, and the pressure was kept for 24 hours.

[0043] Testing: after sample NO.1 and sample NO.2 were taken respectively to be subjected to enzymolysis with amylase in purified water, the content of ethyl alcohol and ethyl acetate in the product was tested respectively through a GC method; the water absorption of sample NO.1 and sample NO.2 was measured by respectively weighing their mass before and after water absorption at saturation; and the initial amount of contaminated bacteria of the samples was detected by 1100 Microbiological Tests of General Requirements of Pharmacopeia Volume IV, and results were as follows.

TABLE-US-00007 Test items Sample NO. 1 Sample NO. 2 Ethyl alcohol residue 0.030% 2.18% Ethyl acetate residue 0.020% 1.02% water absorption  1304% 1280%  Initial amount of ≤10 cfu/g ≤10 cfu/g contaminated bacteria