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Method for efficiently detecting residual solvent in poly-L-lactic acid and preparation thereof

A technology of poly-L-lactic acid and residual solvents, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as differences in solvents and quality control methods, achieve broad prospects for industrialization, good sampling precision, and accurate measurement results reliable effect

Pending Publication Date: 2022-03-04
MEIYAN SPACE (HEBEI) BIOTECHNOLOGY CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

PLLA injection fillers are mostly freeze-dried powder injections, and the dosage form and preparation process are different from cross-linked sodium hyaluronate gel. There are also differences in the preparation and purification of the two solvents and quality control methods

Method used

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  • Method for efficiently detecting residual solvent in poly-L-lactic acid and preparation thereof
  • Method for efficiently detecting residual solvent in poly-L-lactic acid and preparation thereof
  • Method for efficiently detecting residual solvent in poly-L-lactic acid and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Example 1 Preparation of PLLA polymer

[0100] Add 500g of L-lactide to a 2000mL single-necked bottle, and heat it to 130°C under nitrogen protection. After the L-lactide is completely melted, add 0.15g of stannous isooctanoate and 1.5g of lauryl alcohol, and keep warm at 130°C React for 24 hours, after cooling the reaction solution to room temperature, add 1L of dichloromethane, stir to dissolve, filter, transfer the resulting solution to a 50L reaction kettle, add 4L of dichloromethane, dropwise add 25L of methanol, crystallize at room temperature, filter, The filter cake was dried at 50°C to obtain PLLA polymer with a weight average molecular weight of 36,000.

Embodiment 2

[0101] Example 2 Preparation of PLLA polymer

[0102] Add 500g of L-lactide to a 2000mL single-necked bottle, and heat it to 120°C under nitrogen protection. After the L-lactide is completely melted, add 0.1g of stannous chloride and 1.2g of lauryl alcohol, and keep the reaction at 120°C. After 48 hours, after the reaction solution was lowered to room temperature, 1 L of chloroform was added, stirred to dissolve, filtered, the solution was transferred to a 50 L reaction kettle, 4 L of chloroform was added, 25 L of n-heptane was added dropwise, crystallized at room temperature, filtered, The filter cake was dried at 50°C to obtain PLLA polymer with a weight average molecular weight of 39,000.

Embodiment 3

[0103] Example 3 Preparation of PLLA polymer microparticles

[0104] Weigh 200 g of the PLLA polymer prepared in Example 1, add 4 L of tetrahydrofuran, stir to dissolve, slowly add 12 L of anhydrous methanol dropwise, after the dropwise addition, stir for about 1 hour, filter, and rinse the filter cake with anhydrous methanol, Vacuum-dried at 35°C and passed through a 200-mesh sieve to obtain PLLA particles with a heat of fusion of 54.3 J / g, D(3,2) of 21.7 μm, D(4,3) of 32.4 μm, and a maximum particle size of about 66.9 μm.

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Abstract

The invention discloses a gas chromatographic method for a residual solvent in poly-L-lactic acid, which comprises the following steps: taking cyanopropyl phenyl-dimethyl polysiloxane as a stationary phase of a capillary gas chromatographic column, controlling the initial temperature at 35-50 DEG C, heating to 160-280 DEG C at the rate of 5-20 DEG C per minute, keeping the temperature for 3-15 minutes, and injecting a sample; the temperature of a sample inlet is 200-250 DEG C; the temperature of the detector is 220-320 DEG C; the carrier gas is nitrogen, the flow rate is 2.0-5.0 ml / min, the split ratio is (8-15): 1, headspace sampling is performed, the sampling amount is 1-10 ml, and the residual solvent is selected from any one or a combination of methylbenzene, benzene, dichloromethane, trichloromethane, ethanol, acetone, ethyl acetate, normal hexane, cyclohexane, tetrahydrofuran, chloroform, normal heptane, isopropanol and methanol. The method disclosed by the invention is high in sensitivity and good in accuracy, and the residual solvent with strong toxicity in the poly-L-lactic acid can be conveniently controlled within a safety limit range.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for efficiently detecting residual solvents in poly-L-lactic acid and its preparations. Background technique [0002] Injectable fillers (also known as dermal fillers, soft tissue fillers) are mainly used to treat congenital defects and acquired defects, including correcting or even removing deep skin lines, wrinkles, folds and creases, filling and repairing skin depressions, and treating facial defects. lipoatrophy etc. An ideal injectable filler has the following characteristics: ① safe, little damage, good biocompatibility, not easy to infect or induce allograft granuloma; ② good stability, not easy to move, and can maintain a fixed volume and flexibility; ③ not It will be swallowed by phagocytic cells; ④ Effectively promote the regeneration of collagen in the body, naturally and continuously change the facial contour, and increase the elasticity and moisture of the fill...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86G01N30/68
CPCG01N30/02G01N30/06G01N30/8675G01N30/68
Inventor 牛玉乐王宏王晓平郑金敏王爽梁晓东邓声菊刚梁
Owner MEIYAN SPACE (HEBEI) BIOTECHNOLOGY CO LTD
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