KR102466375B1 - Spray drying method of Gwanggwakhyang granules - Google Patents

Spray drying method of Gwanggwakhyang granules Download PDF

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KR102466375B1
KR102466375B1 KR1020207034397A KR20207034397A KR102466375B1 KR 102466375 B1 KR102466375 B1 KR 102466375B1 KR 1020207034397 A KR1020207034397 A KR 1020207034397A KR 20207034397 A KR20207034397 A KR 20207034397A KR 102466375 B1 KR102466375 B1 KR 102466375B1
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spray drying
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바오시엔 장
옌잉 리
신신 리
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베이징 인크리즈팜 코퍼레이션 리미티드
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Abstract

농축된 광곽향 추출물을 취하고 2%~5%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃~180℃, 출구 온도 90℃~95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하는 것을 포함하는 광곽향 과립제의 분무 건조 방법. 상기 농축된 추출물의 60℃에서 상대 밀도는 1.02~1.10이다.Take the concentrated Gwanggwakhyang extract, add 2% to 5% of β-cyclodextrin, mix it evenly, filter it, and spray-dry it at an inlet temperature of 175°C to 180°C and an outlet temperature of 90°C to 95°C to obtain a dry extract powder. A method for spray drying of luminous granules comprising collecting. The relative density at 60° C. of the concentrated extract is 1.02 to 1.10.

Description

광곽향 과립제의 분무 건조 방법Spray drying method of Gwanggwakhyang granules

본 발명은 한방약 과립제 생산기술 분야에 관한 것으로, 보다 자세하게는 개선된 광곽향(廣藿香) 과립제의 분무 건조 방법에 관한 것이며 한방약 생산기술 분야에 속한다.The present invention relates to the field of oriental medicine granule production technology, and more particularly, to an improved method for spray drying of Gwanggwakhyang granules, and belongs to the field of oriental medicine production technology.

한방약 과립제란, 단미(單味) 생약을 추출 농축함으로써 만들어지며 한방약 임상 처방용 과립제를 말한다. 중국에서는 예전에 단미 한방약 농축 과립제라고도 불렸으며 상품명이나 통칭으로는 달이지 않는 한방약 생약, 신생약, 정제 생약, 음료형 생약, 과학 한방약 등도 있다.Oriental medicine granules are made by extracting and concentrating Danmi (單味) crude drugs and refer to granules for clinical prescription of herbal medicines. In China, in the past, it was also called Danmi herbal medicine concentrated granules, and under the brand name or generic name, there are herbal medicines without decoction, new medicines, tablets crude medicines, beverage type herbal medicines, and scientific herbal medicines.

건조 과정은 한방약 과립제 제조에서 중요한 과정 중 하나이다. 한방약 추출물을 건조시키는 방법으로는 예를 들면 진공 건조, 동결 건조, 유동층 건조, 분무 건조 등 많은 방법을 들 수 있다. 그 중에서도 분무 건조는 건조 시간이 짧고 건조 면적이 넓으며 유효성분 파괴가 적은 점 등의 장점을 가져 한방약 액체·반액체 물질의 건조에 이상적인 방법이다.The drying process is one of the important processes in manufacturing herbal medicine granules. As a method of drying the herbal medicine extract, there may be mentioned many methods such as vacuum drying, freeze drying, fluidized bed drying, spray drying, and the like. Among them, spray drying has advantages such as a short drying time, a large drying area, and little destruction of active ingredients, making it an ideal method for drying liquid and semi-liquid substances of oriental medicine.

생약 광곽향은 꿀풀과 식물인 파촐리 Pogostemon cablin(Blanco) Benth.의 지상부를 건조한 것으로 향으로 탁함을 해소하고 비장과 위장의 문제를 다스려 구토를 멎게 하고 더운 기운을 없애는 등의 효능을 가지며, 주로 습탁중조(濕濁中阻), 완비구토, 서습표증(暑濕表證), 습온초기(濕溫初起), 발열권태(發熱倦怠), 흉민불서(胸悶不舒), 한습폐서(寒濕閉暑), 복통토사(腹痛吐瀉), 비연두통(鼻淵頭痛)의 치료에 이용된다.Herbal medicine Gwanggwak incense is a dried above-ground part of the Lamiaceae plant, Patchouli Pogostemon cablin (Blanco) Benth. Mainly wet and wet diarrhea, complete vomiting, suffocation, wet temperature early, fever malaise, poor circulation, poor circulation濕閉暑), abdominal pain and vomiting (腹痛吐瀉), is used for the treatment of nasolacrimal headache (鼻淵頭痛).

광곽향을 한방약 과립제로 사용하는 것은 종래기술이지만 광곽향 과립제 건조 기술에 대해서는 거의 개시되어 있지 않다. 중국특허출원(CN107397787A)에는 짜낸 광곽향 조합액을 40~80℃에서 감압 농축하여 상대 밀도가 1.02~1.10인 농축액을 얻고, 이어서 분무 건조하여 입구 온도를 100~140℃로 하고 출구 온도를 90~120℃로 하는 조건으로 그대로 분무 건조하는, 광곽향 생착즙 분무 건조 과립 음편(飮片)의 제조 과정이 개시되어 있다. CN107397787A에 개시된 방법은 간단하고 조작이 쉽지만 광곽향에 알코올, 케톤, 글리코시드 등의 다양한 성분이 포함되어 있고, 조합액의 점도가 높아 조합액이 분무 건조 중 탑에 부착되는 현상이 발생하여 분무 건조 효율에 크게 악영향을 줄 뿐만 아니라 재료 일부가 손실되어 건조 추출물 분말의 수율이 저하되기도 한다.The use of Gwanggwakhyang as herbal medicine granules is a prior art, but little has been disclosed about the drying technique of Gwanggwakhyang granules. In the Chinese patent application (CN107397787A), the squeezed gwanggwakhyang preparation solution is concentrated under reduced pressure at 40~80℃ to obtain a concentrate having a relative density of 1.02~1.10, and then spray-dried to set the inlet temperature to 100~140℃ and the outlet temperature to 90~ The manufacturing process of Gwanggwak-hyang raw juice spray-dried granular pieces, which is spray-dried as it is under the condition of 120 ° C., is disclosed. The method disclosed in CN107397787A is simple and easy to operate, but various components such as alcohol, ketone, and glycoside are included in the gwanggwak fragrance, and the viscosity of the preparation solution is high, so that the mixture solution adheres to the tower during spray drying. In addition to greatly adversely affecting the efficiency, some of the material is lost and the yield of the dried extract powder is lowered.

본 발명의 목적은 종래기술의 단점을 극복하여 프로세스가 간단하고 공업적 생산에 유리하며 분무 건조 중 벽면 부착 현상의 발생을 효과적으로 방지하면서 한방약 추출물의 분무 건조 공정에서 건조 추출물 분말의 수율을 효과적으로 향상시킬 수 있는 광곽향 한방약 과립제의 분무 건조 프로세스를 제공하는 데 있다.An object of the present invention is to overcome the shortcomings of the prior art, so that the process is simple, advantageous for industrial production, and effectively prevents the occurrence of wall adhesion phenomenon during spray drying, while effectively improving the yield of dry extract powder in the spray drying process of herbal medicine extract. It is to provide a spray drying process for Gwanggwakhyang herbal medicine granules.

상기 과제를 해결하기 위해 본 발명에서 채용하는 구성은 아래와 같다.The configuration employed in the present invention to solve the above problems is as follows.

농축된 광곽향 추출물을 취하고, 이어서 2%~5%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고, 입구 온도 175℃~180℃, 출구 온도 90℃~95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하는 것을 포함하는, 광곽향 한방약 과립제의 분무 건조 방법.Take the concentrated Gwanggwakhyang extract, then add 2% to 5% of β-cyclodextrin, mix it uniformly, filter it, and dry it by spray drying at an inlet temperature of 175°C to 180°C and an outlet temperature of 90°C to 95°C. A spray drying method of Gwanggwakhyang herbal medicine granules, comprising collecting extract powder.

상기 분무 건조 방법의 바람직한 일 실시형태에서는 상기 농축된 추출물의 60℃에서 상대 밀도가 1.02~1.10이고, 바람직하게는 1.03~1.10이다.In a preferred embodiment of the spray drying method, the relative density at 60° C. of the concentrated extract is 1.02 to 1.10, preferably 1.03 to 1.10.

상기 분무 건조 방법의 바람직한 일 실시형태에서는 상기 농축된 추출물의 60℃에서 상대 밀도가 1.05~1.08이다.In a preferred embodiment of the spray drying method, the relative density at 60° C. of the concentrated extract is 1.05 to 1.08.

상기 분무 건조 방법의 바람직한 일 실시형태에서는 추출물에 3%~4%의 β-시클로덱스트린을 첨가한다. 바람직하게는 3%의 β-시클로덱스트린을 첨가한다.In a preferred embodiment of the spray drying method, 3% to 4% of β-cyclodextrin is added to the extract. Preferably 3% of β-cyclodextrin is added.

상기 분무 건조 방법의 바람직한 일 실시형태에서는 분무 건조에서 입구 온도가 175℃이고 출구 온도가 95℃이다.In a preferred embodiment of the spray drying method, the inlet temperature in the spray drying is 175°C and the outlet temperature is 95°C.

상기 분무 건조 방법의 바람직한 일 실시형태에서는 상기 건조 추출물의 수율이 78.02%~96.56%이고, 바람직하게는 78.02%, 81.09%, 81.15%, 84.57%, 95.44% 또는 96.56%이다.In a preferred embodiment of the spray drying method, the yield of the dried extract is 78.02% to 96.56%, preferably 78.02%, 81.09%, 81.15%, 84.57%, 95.44% or 96.56%.

일반적으로 사용되는 계량 방법으로서, 본 발명에서 β-시클로덱스트린의 첨가량은 농축된 광곽향 추출물의 중량을 기준으로 산출한다.As a generally used metering method, in the present invention, the amount of β-cyclodextrin added is calculated based on the weight of the concentrated Gwanggwakhyang extract.

본 발명자는 한방약 과립제의 분무 건조에 대해 예의 연구를 거듭한 결과, 놀랍게도 광곽향 과립제를 제조할 때 광곽향 과립제를 분무 건조시 보조제로서 β-시클로덱스트린을 소량 첨가하면 분무 건조 중 탑에 부착되는 현상을 크게 개선할 수 있어 광곽향 과립제 분무 건조 공정에서 건조 추출물의 수율을 현저하게 향상시킬 수 있음을 발견하였다. 종래기술에서는 통상 β-시클로덱스트린을 관용적인 의약품용 보조제로 인식하여 주로 휘발성 기름의 포접에 사용하는데 분무 건조 보조제로 사용되는 경우는 적다고 생각된다. 소수의 문헌에 그 사용량이 5% 이상인 것이 보고되어 있을 뿐이다. 보조제의 사용량이 지나치게 많으면 처방 과립제에서 주요 제제의 함유량이 영향을 받아 환자의 복용량이 많아질 뿐만 아니라 공업적 생산시에 비용이 증가하는 등 불리한 결과로 이어진다. 또한 본 발명의 출원인은 광곽향 추출물의 상대 밀도도 분무 건조 프로세스 및 건조 추출물의 수율에 큰 영향을 주는 요소 중 하나이며, 상대 밀도가 너무 높거나 너무 낮으면 분무 건조 상황 및 건조 추출물의 수율이 함께 영향을 받지만, 상대 밀도가 적절한 범위라면 분무 건조시 프로세스 제어 및 건조 추출물 분말의 수율에 유리하다는 것을 발견하였다.As a result of repeated research on spray drying of herbal medicine granules, the present inventors surprisingly found that when a small amount of β-cyclodextrin was added as an auxiliary agent during spray drying of Kwanggwakhyang granules, adhesion to the tower during spray drying was observed. It was found that the yield of the dried extract can be significantly improved in the spray drying process of Gwanggwakhyang granules. In the prior art, β-cyclodextrin is generally recognized as an adjuvant for pharmaceuticals and is mainly used for inclusion of volatile oils, but it is considered that it is rarely used as a spray drying aid. Only a few literatures have reported that the amount used is more than 5%. If the amount of the adjuvant is too large, the content of the main agent in the prescription granules is affected, leading to unfavorable results such as an increase in the patient's dose as well as an increase in cost in industrial production. In addition, the applicant of the present invention also stated that the relative density of Gwanggwakhyang extract is also one of the factors that greatly affects the spray drying process and the yield of the dried extract, and if the relative density is too high or too low, the spray drying situation and the yield of the dried extract are together Although affected, it has been found that if the relative density is in an appropriate range, it is advantageous for process control and yield of dry extract powder during spray drying.

이하, 실시예를 통해 본 발명을 더욱 상세하게 설명하지만, 이 실시예들은 본 발명을 설명하기 위한 것에 불과하며 본 발명을 제한하는 것은 아니다.Hereinafter, the present invention will be described in more detail by way of Examples, but these Examples are only for illustrating the present invention and do not limit the present invention.

[실시예 1][Example 1]

상대 밀도가 1.05(60℃)인 농축된 광곽향 추출물을 취하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.05 (60° C.) was taken and spray dried at an inlet temperature of 175° C. and an outlet temperature of 95° C. to collect dry extract powder.

[실시예 2][Example 2]

상대 밀도가 1.05(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 2%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.A concentrated extract of Gwanggwakhyang with a relative density of 1.05 (60°C) was taken, then 2% of β-cyclodextrin was added, mixed uniformly, filtered, and dried by spray drying at an inlet temperature of 175°C and an outlet temperature of 95°C. The powder was collected.

[실시예 3][Example 3]

상대 밀도가 1.05(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 3%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.05 (60°C) was taken, then 3% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract The powder was collected.

[실시예 4][Example 4]

상대 밀도가 1.05(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 4%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.05 (60°C) was taken, then 4% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract The powder was collected.

[실시예 5][Example 5]

상대 밀도가 1.03(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 3%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.03 (60°C) was taken, then 3% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract The powder was collected.

[실시예 6][Example 6]

상대 밀도가 1.08(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 3%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.A concentrated extract of Gwanggwakhyang with a relative density of 1.08 (60°C) was taken, then 3% of β-cyclodextrin was added, mixed uniformly, filtered, and dried by spray drying at an inlet temperature of 175°C and an outlet temperature of 95°C. The powder was collected.

[실시예 7][Example 7]

상대 밀도가 1.10(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 3%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.A concentrated extract of Gwanggwakhyang with a relative density of 1.10 (60°C) was taken, then 3% of β-cyclodextrin was added, mixed uniformly, filtered, and dried by spray drying at an inlet temperature of 175°C and an outlet temperature of 95°C. The powder was collected.

[실시예 8][Example 8]

상대 밀도가 1.01(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 3%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.01 (60°C) was taken, then 3% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract The powder was collected.

[실시예 9][Example 9]

상대 밀도가 1.11(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 3%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.11 (60°C) was taken, then 3% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract The powder was collected.

[실시예 10][Example 10]

상대 밀도가 1.05(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 1.5%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.05 (60°C) was taken, then 1.5% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract. The powder was collected.

[실시예 11][Example 11]

상대 밀도가 1.05(60℃)인 농축된 광곽향 추출물을 취하고, 이어서 6%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고 입구 온도 175℃, 출구 온도 95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하였다.The concentrated Gwanggwakhyang extract having a relative density of 1.05 (60°C) was taken, then 6% of β-cyclodextrin was added, mixed uniformly, filtered, and spray dried at an inlet temperature of 175°C and an outlet temperature of 95°C to dry extract The powder was collected.

분무 건조 상황 및 건조 추출물의 수율 고찰 결과Results of spray drying conditions and yield of dried extracts

실시예Example 분무 건조 상황spray drying situation 건조 추출물의 수율(%)Yield of dry extract (%) 1One 탑에 부착되었고 건조 추출물 분말의 유동성이 나빴다.It adhered to the tower and the dry extract powder had poor flowability. 65.4065.40 22 탑에 약간 부착되었고 건조 추출물 분말의 유동성이 보통이었다.It was slightly adhered to the tower and the flowability of the dry extract powder was moderate. 81.1581.15 33 탑에 부착되지 않았고 건조 추출물 분말의 유동성이 양호하였다.It did not adhere to the tower and the dry extract powder had good fluidity. 95.4495.44 44 탑에 부착되지 않았고 건조 추출물 분말의 유동성이 양호하였다.It did not adhere to the tower and the dry extract powder had good fluidity. 84.5784.57 55 탑에 약간 부착되었고 건조 추출물 분말의 유동성이 보통이었다.It was slightly adhered to the tower and the flowability of the dry extract powder was moderate. 81.0981.09 66 탑에 부착되지 않았고 건조 추출물 분말의 유동성이 양호하였다.It did not adhere to the tower and the dry extract powder had good fluidity. 96.5696.56 77 탑에 약간 부착되었고 건조 추출물 분말의 유동성이 보통이었다.It was slightly adhered to the tower and the flowability of the dry extract powder was moderate. 78.0278.02 88 탑에 부착되었고 건조 추출물 분말의 유동성이 나빴다.It adhered to the tower and the dry extract powder had poor flowability. 70.6570.65 99 탑에 부착되었고 건조 추출물 분말의 유동성이 나빴다.It adhered to the tower and the dry extract powder had poor flowability. 71.1171.11 1010 탑에 부착되었고 건조 추출물 분말의 유동성이 나빴다.It adhered to the tower and the dry extract powder had poor flowability. 72.9772.97 1111 탑에 부착되었고 건조 추출물 분말의 유동성이 나빴다.It adhered to the tower and the dry extract powder had poor flowability. 71.4571.45

고찰 결과에서 알 수 있듯이, 농축 건조 추출물 분말의 상대 밀도, 보조제인 β-시클로덱스트린을 사용하는지, 및 β-시클로덱스트린의 사용량은 분무 건조 프로세스 및 건조 추출물의 수율에 커다란 영향을 끼친다. 상대 밀도가 1.05~1.08이고 β-시클로덱스트린의 사용량이 3% 정도일 때 분무 건조 상황이 가장 좋았으며 건조 추출물의 수율이 가장 높았다.As can be seen from the results of the review, the relative density of the concentrated dry extract powder, whether the auxiliary β-cyclodextrin is used, and the amount of β-cyclodextrin used have a great influence on the spray drying process and the yield of the dried extract. When the relative density was 1.05 to 1.08 and the amount of β-cyclodextrin was about 3%, the spray drying condition was the best and the yield of the dried extract was the highest.

Claims (7)

농축된 광곽향 추출물을 취하고, 이어서 상기 농축된 광곽향 추출물의 중량을 기준으로 3% 내지 4%의 β-시클로덱스트린을 첨가하여 균일하게 혼합하여 여과하고, 입구 온도 175℃~180℃, 출구 온도 90℃~95℃ 조건에서 분무 건조하여 건조 추출물 분말을 수집하는 것을 포함하는 것을 특징으로 하고,
상기 농축된 광곽향 추출물의 60℃에서 상대 밀도가 1.05 내지 1.08인, 광곽향 한방약 과립제의 분무 건조 방법.
Take the concentrated Gwanggwakhyang extract, then add 3% to 4% β-cyclodextrin based on the weight of the concentrated Gwanggwakhyang extract, mix uniformly, and filter, inlet temperature 175°C to 180°C, outlet temperature It is characterized in that it comprises collecting the dry extract powder by spray drying under the conditions of 90 ° C to 95 ° C,
The concentrated Gwanggwakhyang extract has a relative density of 1.05 to 1.08 at 60°C, a spray drying method of Gwanggwakhyang herbal medicine granules.
삭제delete 삭제delete 삭제delete 청구항 1에 있어서,
상기 β-시클로덱스트린을 첨가하는 것은 상기 농축된 광곽향 추출물의 중량을 기준으로 3%의 β-시클로덱스트린을 첨가하는 것인 분무 건조 방법.
The method according to claim 1,
The addition of the β-cyclodextrin is a spray drying method of adding 3% β-cyclodextrin based on the weight of the concentrated Gwanggwakhyang extract.
청구항 1에 있어서,
상기 분무 건조에서는 상기 입구 온도가 175℃이고 상기 출구 온도가 95℃인 분무 건조 방법.
The method according to claim 1,
In the spray drying, the inlet temperature is 175°C and the outlet temperature is 95°C.
청구항 1에 있어서,
건조 추출물의 수율이 95.44% 또는 96.56%인 분무 건조 방법.
The method according to claim 1,
A spray drying method wherein the yield of the dry extract is 95.44% or 96.56%.
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